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CN110250446A - A method for reducing nitrite content in sauced meat products - Google Patents

A method for reducing nitrite content in sauced meat products Download PDF

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CN110250446A
CN110250446A CN201910669202.8A CN201910669202A CN110250446A CN 110250446 A CN110250446 A CN 110250446A CN 201910669202 A CN201910669202 A CN 201910669202A CN 110250446 A CN110250446 A CN 110250446A
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ultrasonic
meat
beef
nitrite
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付丽
高雪琴
申晓琳
张秀凤
杨宝进
郝修振
马微
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Henan University of Animal Husbandry and Economy
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Henan University of Animal Husbandry and Economy
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23BPRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B4/00Preservation of meat, sausages, fish or fish products
    • A23B4/015Preserving by irradiation or electric treatment without heating effect
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23BPRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B4/00Preservation of meat, sausages, fish or fish products
    • A23B4/14Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
    • A23B4/18Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
    • A23B4/20Organic compounds; Microorganisms; Enzymes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L13/00Meat products; Meat meal; Preparation or treatment thereof
    • A23L13/40Meat products; Meat meal; Preparation or treatment thereof containing additives
    • A23L13/42Additives other than enzymes or microorganisms in meat products or meat meals
    • A23L13/428Addition of flavours, spices, colours, amino acids or their salts, peptides, vitamins, yeast extract or autolysate, nucleic acid or derivatives, organic acidifying agents or their salts or acidogens, sweeteners, e.g. sugars or sugar alcohols; Addition of alcohol-containing products
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L13/00Meat products; Meat meal; Preparation or treatment thereof
    • A23L13/70Tenderised or flavoured meat pieces; Macerating or marinating solutions specially adapted therefor
    • A23L13/72Tenderised or flavoured meat pieces; Macerating or marinating solutions specially adapted therefor using additives, e.g. by injection of solutions
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/30Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
    • A23L5/32Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

本发明公开了一种降低酱肉制品中亚硝酸盐含量的方法,包括以下步骤:S1、对牛肉进行腌制,待牛肉腌至颜色完全呈腌肉色或暗红色,结束腌制;S2、将腌制好的牛肉放入容器中,在容器中加入水和复合香辛料提取液,复合香辛料提取液的重量占牛肉与水总重量的1%~5%;S3、对容器内的牛肉进行煮制,同时使用超声波发生器对牛肉进行超声波反应,将超声波的发射频率设定为22kHz~40kHz、将超声波的反应温度设定为75℃~85℃;S4、煮制60min~120min后,关闭超声波发生器,将牛肉捞出,冷却至室温即可。

The invention discloses a method for reducing the content of nitrite in sauced meat products, comprising the following steps: S1, marinating the beef, until the beef is marinated until the color is completely cured meat color or dark red, and then the curing is completed; S2, marinating the beef Put the marinated beef into a container, add water and compound spice extract to the container, the weight of the compound spice extract accounts for 1% to 5% of the total weight of beef and water; S3, cook the beef in the container At the same time, use the ultrasonic generator to perform ultrasonic reaction on the beef, set the ultrasonic emission frequency to 22kHz-40kHz, and set the ultrasonic reaction temperature to 75°C-85°C; S4. After cooking for 60min-120min, turn off the ultrasonic generation Remove the beef from the container and let it cool to room temperature.

Description

一种降低酱肉制品中亚硝酸盐含量的方法A method for reducing nitrite content in sauced meat products

技术领域technical field

本发明涉及食品加工领域,尤其涉及一种降低酱肉制品中亚硝酸盐含量的方法。The invention relates to the field of food processing, in particular to a method for reducing nitrite content in sauced meat products.

背景技术Background technique

酱肉作为中式肉制品中最常见的酱卤肉制品,因为其产品具有的鲜明特点而广泛被人们食用。优质酱肉色泽酱红,油润光亮,肌肉中少量牛筋色黄透明;肉质紧实,切片时完整不松散;吃起来咸淡适中,酱香浓郁,不硬不柴。As the most common stewed meat product in Chinese meat products, sauced meat is widely eaten by people because of its distinctive characteristics. High-quality sauce meat is red in color, oily and bright, and a small amount of beef tendon in the muscle is yellow and transparent; the meat is firm and intact when sliced;

在酱肉的加工过程中,通常会加入亚硝酸盐,主要是使肉制品的色泽呈粉红色,发色原理是肉中存在的肌红蛋白通过与亚硝酸盐的结合,生成了亚硝基肌红蛋白,其对保持肉制品的鲜红色泽有着重要作用。亚硝酸盐不仅具有发色作用,并且对于肉制品的口感、风味都发挥着重要的作用,此外,在抑制微生物的生长方面也有着积极的作用。但是亚硝酸盐的大量摄入对人体是有害的,它作为亚硝胺的前体物质,在食品加工和储藏过程中易转化为N-亚硝基化合物,可致人体中毒甚至有极强的致癌性,对人类健康造成极大危害。现在世界各国对于食品安全性问题变得越来越重视,除了严格的限制亚硝酸盐的使用量之外,如何降低肉制品中亚硝酸盐的含量是食品安全领域急需解决的问题。During the processing of sauced meat, nitrite is usually added, mainly to make the meat product pink in color. The principle of color development is that myoglobin in the meat combines with nitrite to generate nitroso Myoglobin, which plays an important role in maintaining the bright red color of meat products. Nitrite not only has a color development effect, but also plays an important role in the taste and flavor of meat products. In addition, it also plays a positive role in inhibiting the growth of microorganisms. However, a large intake of nitrite is harmful to the human body. As a precursor of nitrosamines, it is easily converted into N-nitroso compounds during food processing and storage, which can cause human poisoning and even strong Carcinogenicity, causing great harm to human health. Now countries around the world are paying more and more attention to food safety issues. In addition to strictly limiting the use of nitrite, how to reduce the content of nitrite in meat products is an urgent problem in the field of food safety.

发明内容Contents of the invention

本发明目的是针对上述问题,提供一种可以有效降低酱肉制品中亚硝酸盐含量的方法。The purpose of the present invention is to address the above problems and provide a method that can effectively reduce the content of nitrite in sauced meat products.

为了实现上述目的,本发明的技术方案是:In order to achieve the above object, technical scheme of the present invention is:

一种降低酱肉制品中亚硝酸盐含量的方法,包括以下步骤:A method for reducing nitrite content in sauced meat products, comprising the following steps:

S1、对牛肉进行腌制,待牛肉腌至颜色完全呈腌肉色或暗红色,结束腌制;S1. Marinate the beef until the beef is marinated until the color is completely cured meat color or dark red, and the marinating is finished;

S2、将腌制好的牛肉放入容器中,在容器中加入水和复合香辛料提取液,复合香辛料提取液的重量占牛肉与水总重量的1%~5%;S2. Put the marinated beef into a container, add water and compound spice extract to the container, the weight of the compound spice extract accounts for 1% to 5% of the total weight of beef and water;

S3、对容器内的牛肉进行煮制,同时使用超声波发生器对牛肉进行超声波反应,将超声波的发射频率设定为22kHz~40kHz、将超声波的反应温度设定为75℃~85℃;S3. Boil the beef in the container, and at the same time use the ultrasonic generator to perform ultrasonic reaction on the beef, set the ultrasonic emission frequency to 22kHz-40kHz, and set the ultrasonic reaction temperature to 75°C-85°C;

S4、煮制60min~120min后,关闭超声波发生器,将牛肉捞出,冷却至室温即可。S4. After cooking for 60 minutes to 120 minutes, turn off the ultrasonic generator, remove the beef, and cool it to room temperature.

进一步的,所述步骤S2中复合香辛料提取液的制备包括以下步骤:Further, the preparation of the compound spice extract in the step S2 includes the following steps:

S21、分别称取八角、桂皮、生姜三种香辛料,将桂皮、八角用粉碎机粉碎至粉状,将生姜洗净、去皮、切碎,备用;S21. Weigh the three spices of star anise, cassia bark and ginger respectively, crush the cinnamon bark and star anise into powder with a pulverizer, wash, peel and chop the ginger, and set aside;

S22、采用醇浸提取法分别对八角、桂皮进行提取;在容器中放入八角或桂皮粉末,加入3倍体积的75%乙醇,40℃下振荡浸泡1h,然后过滤,将滤液收集起来,用旋转蒸发仪在50℃温度下进行浓缩,分别得到八角浓缩液和桂皮浓缩液;S22. Extract star anise and cassia bark respectively by alcohol extraction; put star anise or cassia bark powder in a container, add 3 times the volume of 75% ethanol, shake and soak at 40°C for 1 hour, then filter, collect the filtrate, and use The rotary evaporator is concentrated at a temperature of 50°C to obtain star anise concentrate and cinnamon concentrate respectively;

S23、采用水浸提取法对生姜进行提取;在容器中放入切碎的生姜,加3倍体积的蒸馏水,40℃下振荡浸泡1h,然后过滤,将滤液收集起来,用旋转蒸发仪在64℃温度下进行浓缩,得到生姜浓缩液;S23. Extract ginger by water immersion extraction; put chopped ginger in a container, add 3 times the volume of distilled water, shake and soak at 40°C for 1h, then filter, collect the filtrate, and use a rotary evaporator at 64 Concentrate at a temperature of 10°C to obtain a ginger concentrate;

S24、将八角浓缩液、桂皮浓缩液、生姜浓缩液按1:1:2的比例进行混合,得到复合香辛料提取液。S24. Mix the star anise concentrate, cinnamon concentrate, and ginger concentrate in a ratio of 1:1:2 to obtain a compound spice extract.

进一步的,所述步骤S2中复合香辛料提取液的重量占牛肉与水总重量的1%。Further, the weight of the compound spice extract in the step S2 accounts for 1% of the total weight of beef and water.

进一步的,所述步骤S3中超声波的发射频率设定为40kHz、将超声波的反应温度设定为80℃。Further, in the step S3, the transmission frequency of the ultrasonic wave is set to 40 kHz, and the reaction temperature of the ultrasonic wave is set to 80°C.

进一步的,所述步骤S4中煮制时间设定为100min。Further, the cooking time in the step S4 is set to 100min.

与现有技术相比,本发明具有的优点和积极效果是:Compared with prior art, the advantages and positive effects that the present invention has are:

本发明通过采用复合香辛料提取液和超声波相结合的方式进行煮制牛肉,有效降低了酱肉制作过程中残留的亚硝酸盐含量,其亚硝酸盐清除率达到了53.94%,避免了大量的亚硝酸盐进入人体导致出现人体中毒等状况,使得人们可以放心大胆的对酱肉进行食用;并且通过本发明制备出的酱肉具有极好的抗氧化效果,延长了酱肉存储时间的同时保证了酱肉的原汁原味,提高了酱肉的食用效果;另一方面,本发明可以给其他肉类产品降低亚硝酸盐含量的作出提示,从而给食品安全领域作出极大的贡献。In the present invention, the beef is boiled by combining the compound spice extract and ultrasonic waves, which effectively reduces the residual nitrite content in the process of making sauced meat, and its nitrite removal rate reaches 53.94%, avoiding a large amount of nitrite. Nitrate entering the human body leads to human poisoning and other conditions, so that people can safely and boldly eat the sauced meat; and the sauced meat prepared by the present invention has an excellent antioxidant effect, prolonging the storage time of the sauced meat while ensuring The original flavor of the sauced meat improves the edible effect of the sauced meat; on the other hand, the present invention can give hints for reducing the nitrite content of other meat products, thereby making a great contribution to the field of food safety.

附图说明Description of drawings

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. For those skilled in the art, other drawings can also be obtained according to these drawings without any creative effort.

图1为不同超声频率处理酱肉亚时硝酸钠含量变化;Figure 1 is the change of sodium nitrate content in sauce meat treated with different ultrasonic frequencies;

图2为不同超声频率处理酱肉时色差的变化;Figure 2 is the change of color difference when different ultrasonic frequencies are used to process sauced meat;

图3为不同超声频率处理酱肉时过氧化值的含量变化;Fig. 3 is the content variation of peroxide value when different ultrasonic frequencies are processed;

图4为不同超声频率处理酱肉时羰基价变化;Figure 4 shows the change of carbonyl value when different ultrasonic frequencies are used to treat sauce meat;

图5为不同超声温度处理酱肉时亚硝酸钠含量变化;Fig. 5 is the change of sodium nitrite content when different ultrasonic temperatures are processed;

图6为不同超声温度处理酱肉时色差的变化;Fig. 6 is the change of color difference when different ultrasonic temperatures are processed;

图7为不同超声温度处理酱肉时过氧化值的含量变化;Fig. 7 is the content change of peroxide value when different ultrasonic temperatures are processed sauce meat;

图8为不同超声温度处理酱肉时羰基价变化;Figure 8 is the change of carbonyl value when different ultrasonic temperatures are used to treat sauce meat;

图9为不同超声时间处理酱肉时亚硝酸钠含量变化;Fig. 9 is the change of sodium nitrite content when different ultrasonic time is processed sauce meat;

图10为不同超声时间处理酱肉时色差的变化;Fig. 10 is the change of color difference when different ultrasonic time is processed sauce meat;

图11为不同超声时间处理酱肉时过氧化值的含量变化;Fig. 11 is the content change of peroxide value when different ultrasonic time is processed sauce meat;

图12为不同超声时间处理酱肉时羰基价变化;Figure 12 is the change of carbonyl value when different ultrasonic time is used to treat sauce meat;

图13为不同量香辛料提取液处理酱肉时亚硝酸钠含量变化;Fig. 13 is the change of sodium nitrite content when different amounts of spice extracts are processed;

图14为不同量香辛料提取液处理酱肉时色差的变化;Fig. 14 is the change of color difference when different amounts of spice extracts are processed;

图15为不同量香辛料提取液处理酱肉时过氧化值的含量变化;Fig. 15 is the content change of peroxide value when different amounts of spice extracts are processed;

图16为不同量香辛料提取液处理酱肉时羰基价变化;Figure 16 is the variation of carbonyl value when different amounts of spice extracts are used to process sauced meat;

图17为香辛料不同提取方法对亚硝酸盐清除率的变化;Fig. 17 is the change of the different extraction methods of spices to the nitrite scavenging rate;

图18为三种香辛料提取液的不同添加量对亚硝酸盐清除率的变化。Figure 18 shows the change of nitrite removal rate with different additions of three kinds of spice extracts.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative work, any modifications, equivalent replacements, improvements, etc., shall be included in the protection scope of the present invention Inside.

下面通过各项试验对本发明的效果进行验证,本试验以亚硝酸盐含量为主要测定指标,试验超声处理辅助香辛料对酱肉中亚硝酸盐消除效果,优化工艺条件及参数。The effect of the present invention is verified by various tests below. This test takes the nitrite content as the main measurement index, and tests the ultrasonic treatment auxiliary spices on the elimination effect of nitrite in the sauce meat, and optimizes the process conditions and parameters.

试验的主要内容The main content of the test

试验不同超声条件辅助不同量香辛料对酱肉中亚硝酸盐清除效果Test the scavenging effect of different amounts of spices on nitrite in sauced meat under different ultrasonic conditions

以亚硝酸盐腌制的牛肉加工的酱肉为试验对象,将生姜、桂皮、八角三种香辛料按2:1:1复合,采用不同的超声波频率(22kHz、28kHz、40kHz)、超声温度(75℃、80℃、85℃)、超声时间(80min、90min、100min)及不同香辛料添加量(1%、2%、3%、4%、5%)处理肉样,以添加香辛料煮制而不经超声波处理的腌制肉样为对照组1,以清水煮制且不经超声波处理的肉样为对照组2。通过测定亚硝酸钠含量、色差、POV、羰基价等指标,试验不同超声处理条件及不同香辛料提取液添加量对酱肉中亚硝酸盐的清除效果。The sauce meat processed with nitrite-cured beef was used as the test object, and the three spices of ginger, cinnamon and star anise were compounded at a ratio of 2:1:1, and different ultrasonic frequencies (22kHz, 28kHz, 40kHz), ultrasonic temperatures (75 ℃, 80°C, 85°C), ultrasonic time (80min, 90min, 100min) and different spices added (1%, 2%, 3%, 4%, 5%) to treat the meat samples, so that the spices can be added without cooking. The marinated meat sample treated with ultrasonic was the control group 1, and the meat sample boiled in water without ultrasonic treatment was the control group 2. By measuring the sodium nitrite content, color difference, POV, carbonyl value and other indicators, the scavenging effect of different ultrasonic treatment conditions and different spice extracts on the removal of nitrite in sauced meat was tested.

优化超声处理辅助香辛料清除酱肉中亚硝酸盐工艺条件及参数Optimizing the process conditions and parameters of ultrasonic treatment-assisted spices to remove nitrite from sauce meat

根据单因素试验结果,以超声时间、超声频率、超声温度、香辛料提取液添加量为试验因素,以亚硝酸钠含量为测定指标,进行超声波处理辅助香辛料对酱肉中亚硝酸盐清除效果优化,选出最适工艺条件及参数。According to the results of the single factor test, with ultrasonic time, ultrasonic frequency, ultrasonic temperature, and the amount of spice extract added as the experimental factors, and the content of sodium nitrite as the measurement index, ultrasonic treatment was carried out to assist spices in optimizing the removal effect of nitrite in sauced meat. Select the optimum process conditions and parameters.

材料与方法Materials and Methods

材料:Material:

牛腱肉:由河南伊赛牛肉股份有限公司和郑州双汇集团提供;Beef tendon: provided by Henan Yisai Beef Co., Ltd. and Zhengzhou Shuanghui Group;

食盐、亚硝酸钠:由河南牧业经济学院畜产品试验室提供;Salt and sodium nitrite: provided by the Animal Products Laboratory of Henan University of Animal Husbandry and Economics;

香辛料(生姜、桂皮、八角):由河南牧业经济学院畜产品试验室提供;Spices (ginger, cinnamon, star anise): provided by the Animal Products Laboratory of Henan College of Animal Husbandry and Economics;

化学试剂:由天津永大化学试剂公司提供。Chemical reagents: provided by Tianjin Yongda Chemical Reagent Company.

仪器与设备Instruments and Equipment

本试验所用主要仪器与设备见表1。The main instruments and equipment used in this experiment are listed in Table 1.

表1主要仪器与设备Table 1 Main instruments and equipment

酱肉的操作要点Operation points of sauce meat

⑴原料肉的选择;选择符合卫生要求的新鲜牛腱肉。⑴ Selection of raw meat; choose fresh beef tendon meat that meets hygienic requirements.

⑵原料肉的处理与修整;用刀具除去筋膜、筋腱、软骨、脂肪等多余物,将肉块切成300g左右,用清水冲洗干净,水分沥干后备用。⑵Processing and trimming of raw meat; remove fascia, tendons, cartilage, fat and other excess with a knife, cut the meat into about 300g, rinse with clean water, drain the water and set aside.

⑶配料;按配方称取所需香辛料和辅料。(3) Ingredients: Weigh the required spices and auxiliary materials according to the formula.

⑷干腌;将配料称好后,加入盐和硝水,搅拌均匀,置于0~4℃条件下腌制24h。待牛肉腌至其内部颜色完全呈腌肉色或暗红色,腌制结束。(4) Dry salting: After weighing the ingredients, add salt and nitrate, stir well, and marinate at 0-4°C for 24 hours. When the beef is marinated until its internal color is completely bacon color or dark red, the marinating is over.

⑸煮制;对照组:锅内加入适量清水,先将配制好的香辛料提取液放入锅中煮开,然后将腌制好的牛肉放入烧开的锅中,撇除表面浮沫及杂物等。开锅后,沸水煮制30~40min至肉中心温度达72℃以上,捞出肉块,冷却至室温。⑸Cooking; control group: add appropriate amount of water into the pot, first put the prepared spice extract into the pot and boil, then put the marinated beef into the boiling pot, skim off the surface foam and miscellaneous things etc. After boiling, cook in boiling water for 30-40 minutes until the temperature of the center of the meat reaches above 72°C, remove the meat and cool to room temperature.

处理组:将腌制好的牛肉放入玻璃烧杯中,加入水及复合香辛料提取液,然后将玻璃烧杯放入超声波仪器中,设置一定的超声波参数煮制牛肉。待牛肉煮好后,捞出肉块,冷却至室温。Treatment group: Put marinated beef into a glass beaker, add water and compound spice extract, then put the glass beaker into an ultrasonic instrument, set certain ultrasonic parameters to cook the beef. When the beef is cooked, remove the meat and let it cool to room temperature.

⑹冷却、包装;煮制入味后的牛肉,经冷却后进行包装。⑹Cooling and packaging; the cooked beef is packaged after cooling.

⑺成品入库;将成品放入0~4℃冷藏室中保存。⑺The finished product is stored in the warehouse; the finished product is stored in a refrigerator at 0-4°C.

基础配方Basic formula

牛腱肉、食盐2.5%、亚硝酸钠0.015%、香辛料提取液(复合)3%Beef tendon, salt 2.5%, sodium nitrite 0.015%, spice extract (compound) 3%

香辛料提取液的制备Preparation of spice extract

⑴香辛料的预处理⑴ Pretreatment of spices

分别称取300g八角、桂皮、生姜三种香辛料。桂皮、八角用粉碎机粉碎至粉状,留取备用。生姜洗净、去皮、切碎,留取备用。Take by weighing three kinds of spices of 300g star anise, cassia bark, ginger respectively. Cinnamon and star anise are crushed into powder with a grinder, and set aside for later use. Wash the ginger, peel it, chop it, and keep it for later use.

⑵香辛料的提取及浓缩⑵ Extraction and concentration of spices

采用醇浸提取法对八角、桂皮两种香辛料进行提取。称取250g香辛料干粉,放入1000mL锥形瓶中,加750mL75%乙醇40℃下振荡浸泡1h,然后过滤,将滤液收集起来,用旋转蒸发仪50℃浓缩至250mL于250mL容量瓶中备用。Two spices, star anise and cinnamon bark, were extracted by alcohol extraction. Weigh 250g of dry spice powder, put it into a 1000mL conical flask, add 750mL of 75% ethanol and shake and soak at 40°C for 1h, then filter, collect the filtrate, concentrate it to 250mL with a rotary evaporator at 50°C, and put it in a 250mL volumetric flask for later use.

采用水浸提取法对生姜香辛料进行提取。称取250g切碎的生姜,放入1000mL锥形瓶中,加750mL蒸馏水40℃下振荡浸泡1h,然后过滤,将滤液收集起来,用旋转蒸发仪64℃浓缩至250mL于250mL容量瓶中备用。Ginger spices were extracted by water immersion extraction. Weigh 250g of chopped ginger, put it into a 1000mL Erlenmeyer flask, add 750mL of distilled water, shake and soak at 40°C for 1h, then filter, collect the filtrate, concentrate it to 250mL with a rotary evaporator at 64°C, and put it in a 250mL volumetric flask for later use.

⑶香辛料提取液的配制(三种香辛料复配)⑶ Preparation of spice extract (combination of three spices)

分别吸取各香辛料的不同量提取液(八角:桂皮:生姜=1:1:2)置于250mL容量瓶中,混匀。Take different amounts of extracts of each spice (star anise: cinnamon: ginger = 1:1:2) and place them in a 250mL volumetric flask, and mix well.

优化超声处理辅助香辛料清除酱肉中亚硝酸盐工艺条件及参数Optimizing the process conditions and parameters of ultrasonic treatment-assisted spices to remove nitrite from sauce meat

根据单因素试验结果,选取超声频率、超声温度、超声时间和香辛料提取液添加量为试验因素。按四因素三水平安排表(表2)进行复配,以亚硝酸盐含量为测定指标,进行超声波处理辅助香辛料对酱肉中残留亚硝酸盐的消除效果工艺条件及参数的优化。According to the single factor test results, the ultrasonic frequency, ultrasonic temperature, ultrasonic time and the amount of spice extract were selected as the experimental factors. According to the arrangement table of four factors and three levels (Table 2), the compounding was carried out, and the nitrite content was used as the measurement index to optimize the technological conditions and parameters of the elimination effect of ultrasonic treatment assisted spices on residual nitrite in sauced meat.

表2正交试验因素水平安排表Table 2 Orthogonal test factor level arrangement table

亚硝酸盐的测定Determination of nitrite

亚硝酸盐的测定方法采用国标GB5009.33-2016《食品中亚硝酸盐与硝酸盐的测定》第二法分光光度法。The determination method of nitrite adopts the second spectrophotometric method of the national standard GB5009.33-2016 "Determination of nitrite and nitrate in food".

色差的测定Determination of color difference

取包装好的酱肉,用洁净的刀从中切开,取2cm厚的平整断面放于平整操作台上。使用色差计,采用C光源进行色差测量,记录样品的亮度值(L*)、红度值(a*)和黄度值(b*)。Take the packaged sauced meat, cut it with a clean knife, take a 2cm thick flat section and place it on a flat operating table. Use the color difference meter to measure the color difference with C light source, and record the brightness value (L*), redness value (a*) and yellowness value (b*) of the sample.

过氧化值的测定(POV)Determination of peroxide value (POV)

过氧化值的测定方法采用GB5009.277-2016《食品中过氧化值的测定》第一法滴定法。The determination method of peroxide value adopts the first method titration method of GB5009.277-2016 "Determination of peroxide value in food".

羰基价的测定Determination of carbonyl value

羰基价的测定方法采用GB5009.230-2016《食品中羰基价的测定》规定的方法。The determination method of carbonyl value adopts the method stipulated in GB5009.230-2016 "Determination of carbonyl value in food".

亚硝胺的测定Determination of nitrosamines

亚硝胺的测定方法参照国标GB5009.26-2016《食品中N-亚硝胺类化合物的测定》第一法气相色谱-质谱法。The determination method of nitrosamines refers to the first method of gas chromatography-mass spectrometry in the national standard GB5009.26-2016 "Determination of N-nitrosamines in food".

每项指标均取不同处理组的肉样3组,重复测定三次,结果表示为平均值±标准差。采用SigmaPlot10.0软件绘图,采用SPSSStatistics25.0统计分析软件中的独立样本t检验法进行数据的显著性分析。Three groups of meat samples from different treatment groups were taken for each index, and the measurement was repeated three times, and the results were expressed as mean ± standard deviation. SigmaPlot10.0 software was used for drawing, and the independent sample t test method in SPSSStatistics25.0 statistical analysis software was used to analyze the significance of data.

不同超声频率处理对酱肉中亚硝酸盐消除效果试验Experiment on the Elimination Effect of Different Ultrasonic Frequency Treatment on Nitrite in Sauce Meat

以亚硝酸盐腌制的牛肉加工的酱肉为试验对象,将生姜、桂皮、八角复合提取液按肉与水总重的3%的量加入水中进行煮制牛肉,将处理好的原料肉分为5组。超声功率设定为300W、时间为60min、温度为75℃,分别采用22kHz、28kHz、40kHz三个超声频率煮制牛肉,以添加香辛料煮制而不经超声波处理的腌制肉样为对照组1,以清水煮制且不经超声波处理的肉样为对照组2,测定煮制前后肉样中亚硝酸盐的残留量及亚硝胺的含量等指标,试验不同超声波频率对酱肉中残留亚硝酸盐消除效果及亚硝胺的阻断效率。With nitrite-cured beef processed sauce meat as the test object, ginger, cinnamon, star anise compound extract solution was added into water to boil the beef according to the amount of 3% of the total weight of meat and water, and the processed raw meat was divided into For 5 groups. The ultrasonic power was set at 300W, the time was 60min, and the temperature was 75°C. Three ultrasonic frequencies of 22kHz, 28kHz, and 40kHz were used to cook beef respectively. The marinated meat samples cooked with spices without ultrasonic treatment were used as the control group 1 , the meat samples boiled in clear water without ultrasonic treatment were used as the control group 2, the residual nitrite and nitrosamine content in the meat samples before and after cooking were measured, and the effects of different ultrasonic frequencies on the residual nitrosamines in sauced meat were tested. Nitrate elimination effect and nitrosamine blocking efficiency.

不同超声频率条件下酱肉亚硝酸盐含量的变化见图1;The change of nitrite content in sauce meat under different ultrasonic frequency conditions is shown in Figure 1;

由图1可知,对照1组肉样的亚硝酸钠含量为0.0933mg/kg,显著低于对照2组(P<0.05),说明添加香辛料煮制酱肉具有明显的清除亚硝酸盐的效果。超声处理组肉样的亚硝酸钠含量显著低于两个对照组(P<0.05)。超声处理组中,随着超声频率的增大,肉样中亚硝酸钠含量呈先降低后上升的趋势,以28kHz超声处理组肉样的亚硝酸钠含量最低(P<0.05)。It can be seen from Figure 1 that the sodium nitrite content of meat samples in control group 1 was 0.0933 mg/kg, which was significantly lower than that in control group 2 (P<0.05), indicating that adding spices to cook sauced meat has a significant effect of scavenging nitrite. The content of sodium nitrite in the ultrasonic treatment group was significantly lower than that in the two control groups (P<0.05). In the ultrasonic treatment group, as the ultrasonic frequency increased, the sodium nitrite content in the meat samples first decreased and then increased, and the sodium nitrite content in the meat samples was the lowest in the 28kHz ultrasonic treatment group (P<0.05).

不同超声频率条件下酱肉a*值的变化见图2;The change of a* value of sauce meat under different ultrasonic frequency conditions is shown in Figure 2;

由图2可知,对照1组肉样的a*值与对照2组非常接近,差异不显著(P>0.05),说明不经超声波处理添加香辛料煮制肉样对a*值影响不明显。超声组肉样的a*值显著低于两个对照组(P<0.05),一方面原因是经超声波处理后肌肉中的含水量增加,降低了肌肉中色素的浓度,此外,超声波产生的空化效应使肌束变得松散,结缔组织吸水膨胀,其中部分色素溶出,红度下降;另一方面原因是a*值大小与肌肉中血红蛋白、肌红蛋白的含量有关,在一定超声强度下,肉样中残存的淤血更容易流出,肌红蛋白转化得更快。超声处理组中,随着超声频率的增大,肉样的a*值呈先降低后上升的趋势,以28kHz超声处理组肉样的a*值最低(P<0.05)。当超声频率增大到40kHz时a*值上升的原因可能是超声强度过大,导致肉样中的细胞大量破裂,胞内色素释放,使a*值上升。It can be seen from Figure 2 that the a* value of the meat samples in the control group 1 is very close to that of the control group 2, and the difference is not significant (P>0.05), indicating that cooking the meat samples without ultrasonic treatment and adding spices has no obvious effect on the a* value. The a* value of the meat samples in the ultrasonic group was significantly lower than that of the two control groups (P<0.05). On the one hand, the water content in the muscle increased after ultrasonic treatment, which reduced the concentration of pigment in the muscle. In addition, the space produced by ultrasonic The chemical effect makes the muscle bundles loose, the connective tissue absorbs water and swells, some of the pigments dissolve out, and the redness decreases; on the other hand, the reason is that the a* value is related to the content of hemoglobin and myoglobin in the muscle. The remaining blood in the meat sample is easier to flow out, and the conversion of myoglobin is faster. In the ultrasonic treatment group, as the ultrasonic frequency increased, the a* value of the meat samples first decreased and then increased, and the a* value of the meat samples in the 28kHz ultrasonic treatment group was the lowest (P<0.05). When the ultrasonic frequency increases to 40kHz, the reason for the increase of a* value may be that the ultrasonic intensity is too high, which causes a large number of cells in the meat sample to rupture, and the intracellular pigment is released, which increases the a* value.

不同超声频率条件下酱肉的POV含量变化见图3;The changes of POV content of sauce meat under different ultrasonic frequency conditions are shown in Figure 3;

由图3可知,对照1组肉样的POV含量为0.0745g/100g,显著低于对照2组(P<0.05),说明香辛料具有明显的抗氧化效果。超声处理组肉样的POV含量显著低于两个对照组(P<0.05),说明超声波处理促进了香辛料发挥抗氧化作用。超声处理组中,随着超声频率的增大,肉样的POV含量呈先降低后上升的趋势,以28kHz超声处理组肉样的POV含量最低(P<0.05)。当超声频率增大到40kHz时POV含量有所上升,一方面原因可能是高强度的超声处理会显著增加牛肉的蛋白质氧化及脂肪氧化程度;另一方面原因可能是一定浓度的食盐可促进脂质的氧化作用。当食盐浓度增大,过氧化值也增大。超声波对食盐渗透有促进作用。当超声强度增强,食盐浓度增大,过氧化值也增大。It can be seen from Figure 3 that the POV content of meat samples in control group 1 was 0.0745g/100g, which was significantly lower than that in control group 2 (P<0.05), indicating that spices have obvious antioxidant effects. The POV content of meat samples in the ultrasonic treatment group was significantly lower than that of the two control groups (P<0.05), indicating that ultrasonic treatment promoted the antioxidant effect of spices. In the ultrasonic treatment group, with the increase of ultrasonic frequency, the POV content of meat samples first decreased and then increased, and the POV content of meat samples in the 28kHz ultrasonic treatment group was the lowest (P<0.05). When the ultrasonic frequency increases to 40kHz, the POV content increases. On the one hand, the reason may be that high-intensity ultrasonic treatment will significantly increase the degree of protein oxidation and fat oxidation of beef; on the other hand, the reason may be that a certain concentration of salt can promote lipid oxidation. of oxidation. When the salt concentration increases, the peroxide value also increases. Ultrasound can promote the penetration of salt. When the ultrasonic intensity increases, the salt concentration increases, and the peroxide value also increases.

不同超声频率条件下酱肉的羰基价含量变化见图4;The change of carbonyl value content of sauce meat under different ultrasonic frequency conditions is shown in Figure 4;

由图4可知,对照2组肉样的羰基价稍高于对照1组,但差异不显著(P>0.05)。超声处理组肉样的羰基价显著低于两个对照组(P<0.05)。超声处理组中,随着超声频率的增大,肉样中的羰基价呈先降低后上升的趋势,以28kHz超声处理组肉样的羰基价最低(P<0.05)。与图3趋势基本一致。It can be seen from Figure 4 that the carbonyl value of meat samples in control group 2 was slightly higher than that in control group 1, but the difference was not significant (P>0.05). The carbonyl value of meat samples in the ultrasonic treatment group was significantly lower than that of the two control groups (P<0.05). In the ultrasonic treatment group, with the increase of the ultrasonic frequency, the carbonyl value of the meat samples first decreased and then increased, and the carbonyl value of the meat samples was the lowest in the 28kHz ultrasonic treatment group (P<0.05). The trend is basically consistent with that in Figure 3.

不同超声温度处理对酱肉中亚硝酸盐消除效果试验Effect of different ultrasonic temperature treatment on the elimination of nitrite in sauce meat

以亚硝酸盐腌制的牛肉加工的酱肉为试验对象,将生姜、桂皮、八角复合提取液按肉与水总重的3%的量加入水中进行煮制牛肉,将处理好的原料肉分为5组。超声功率设定为300W、时间为60min、频率为28kHz,选择75℃、80℃、85℃三个温度煮制牛肉,以添加香辛料煮制而不经超声波处理的腌制肉样为对照组1,以清水煮制且不经超声波处理的肉样为对照组2,测定煮制前后肉样中亚硝酸盐的残留量及亚硝胺的含量等指标,试验不同超声温度对酱肉中残留亚硝酸盐消除效果及亚硝胺的阻断效率。With nitrite-cured beef processed sauce meat as the test object, ginger, cinnamon, star anise compound extract solution was added into water to boil the beef according to the amount of 3% of the total weight of meat and water, and the processed raw meat was divided into For 5 groups. The ultrasonic power was set to 300W, the time was 60min, and the frequency was 28kHz. Three temperatures of 75°C, 80°C, and 85°C were selected to cook beef. The marinated meat samples cooked with spices without ultrasonic treatment were used as the control group 1 , take the meat samples boiled in clear water without ultrasonic treatment as the control group 2, measure the residual nitrite and nitrosamine content in the meat samples before and after cooking, and test the effect of different ultrasonic temperatures on the residual nitrite in sauced meat. Nitrate elimination effect and nitrosamine blocking efficiency.

不同超声温度条件下酱肉亚硝酸盐含量的变化见图5;The change of nitrite content in sauce meat under different ultrasonic temperature conditions is shown in Figure 5;

由图5可知,对照1组肉样的亚硝酸钠含量为0.114mg/kg,显著低于对照2组(P<0.05)。超声处理组肉样的亚硝酸钠含量显著低于两个对照组(P<0.05)。超声处理组中,随着超声温度的增大,肉样中的亚硝酸钠含量呈先降低后上升的趋势,以80℃超声处理组肉样的亚硝酸钠含量最低(P<0.05)。It can be seen from Figure 5 that the sodium nitrite content of the meat samples in the control group 1 was 0.114 mg/kg, which was significantly lower than that in the control group 2 (P<0.05). The content of sodium nitrite in the ultrasonic treatment group was significantly lower than that in the two control groups (P<0.05). In the ultrasonic treatment group, as the ultrasonic temperature increased, the sodium nitrite content in the meat samples first decreased and then increased, and the sodium nitrite content in the meat samples was the lowest in the ultrasonic treatment group at 80°C (P<0.05).

不同超声波温度条件下酱肉a*值的变化见图6;The change of a* value of sauce meat under different ultrasonic temperature conditions is shown in Figure 6;

由图6可知,对照1组肉样的a*值稍低于对照2组,但差异不显著(P>0.05)。超声组肉样的a*值显著低于两个对照组(P<0.05)。超声处理组中,随着超声温度的增大,肉样的a*值呈先降低后上升的趋势,以80℃超声处理组肉样的a*值最低(P<0.05)。当超声温度上升到85℃,肉样a*值变大,可能是因为超声温度过高,肉样中的细胞大量破裂,胞内色素释放,使a*值上升。It can be seen from Figure 6 that the a* value of meat samples in control group 1 was slightly lower than that in control group 2, but the difference was not significant (P>0.05). The a* value of the meat sample in the ultrasound group was significantly lower than that in the two control groups (P<0.05). In the ultrasonic treatment group, as the ultrasonic temperature increased, the a* value of the meat samples first decreased and then increased, and the a* value of the meat samples in the ultrasonic treatment group at 80°C was the lowest (P<0.05). When the ultrasonic temperature rose to 85°C, the a* value of the meat sample increased, probably because the ultrasonic temperature was too high, a large number of cells in the meat sample ruptured, and the intracellular pigment was released, which increased the a* value.

不同超声温度条件下酱肉的POV含量变化见图7;The change of POV content of sauce meat under different ultrasonic temperature conditions is shown in Figure 7;

由图7可知,对照1组肉样的POV含量为0.119g/100g,显著低于对照2组(P<0.05)。超声处理组肉样的POV含量显著低于两个对照组(P<0.05)。超声处理组中,随超声温度的增加,肉样中POV含量呈先减少后增大的趋势,以80℃超声处理组肉样的POV含量最低(P<0.05)。当超声温度增大到85℃时POV含量有所上升,原因可能是超声温度过高会加速肉样中蛋白质分解,促进脂肪的分解和氧化作用。It can be seen from Figure 7 that the POV content of meat samples in control group 1 was 0.119g/100g, which was significantly lower than that in control group 2 (P<0.05). The POV content of meat samples in the ultrasonic treatment group was significantly lower than that of the two control groups (P<0.05). In the ultrasonic treatment group, with the increase of ultrasonic temperature, the POV content in the meat samples first decreased and then increased, and the POV content of the meat samples in the ultrasonic treatment group at 80°C was the lowest (P<0.05). When the ultrasonic temperature increased to 85°C, the POV content increased. The reason may be that too high ultrasonic temperature will accelerate the decomposition of protein in meat samples, and promote the decomposition and oxidation of fat.

不同超声温度条件下酱肉的羰基价含量变化见图8;The change of carbonyl value content of sauce meat under different ultrasonic temperature conditions is shown in Figure 8;

由图8可知,对照2组肉样的羰基价稍高于对照1组,但差异不显著(P>0.05)。超声处理组肉样的羰基价显著低于两个对照组(P<0.05)。超声处理组中,随超声温度的增加,肉样的羰基价呈先减少后增大的趋势,以80℃超声处理组肉样的羰基价最低(P<0.05)。与图7趋势基本一致。It can be seen from Figure 8 that the carbonyl value of meat samples in control group 2 was slightly higher than that in control group 1, but the difference was not significant (P>0.05). The carbonyl value of meat samples in the ultrasonic treatment group was significantly lower than that of the two control groups (P<0.05). In the ultrasonic treatment group, with the increase of ultrasonic temperature, the carbonyl value of meat samples first decreased and then increased, and the carbonyl value of meat samples in the ultrasonic treatment group at 80°C was the lowest (P<0.05). The trend is basically consistent with that in Figure 7.

不同超声时间处理对酱肉中亚硝酸盐消除效果试验Experiment on the Elimination Effect of Nitrite in Sauce Meat Treated by Different Ultrasonic Time

以亚硝酸盐腌制的牛肉加工的酱肉为试验对象,将生姜、桂皮、八角复合提取液按肉与水总重的3%的量加入水中进行煮制牛肉,将处理好的原料肉分为5组。在超声功率300W、频率28kHz、温度75℃下分别超声波处理60min、90min、120min,以添加香辛料煮制而不经超声波处理的腌制肉样为对照组1,以清水煮制且不经超声波处理的肉样为对照组2,测定煮制前后肉样中亚硝酸盐的残留量及亚硝胺的含量等指标,试验不同超声波处理时间对酱肉中残留亚硝酸盐消除效果及亚硝胺的阻断效率。With nitrite-cured beef processed sauce meat as the test object, ginger, cinnamon, star anise compound extract solution was added into water to boil the beef according to the amount of 3% of the total weight of meat and water, and the processed raw meat was divided into For 5 groups. Ultrasonic treatment at 300W ultrasonic power, frequency 28kHz, and temperature 75°C for 60min, 90min, and 120min, respectively. The marinated meat samples cooked with spices and not treated with ultrasonic were used as control group 1, boiled in water without ultrasonic treatment The meat sample was used as the control group 2, the residual nitrite and nitrosamine content in the meat sample before and after cooking were measured, and the effects of different ultrasonic treatment times on the elimination of residual nitrite and nitrosamine in sauced meat were tested. blocking efficiency.

不同超声时间条件下酱肉亚硝酸盐含量的变化见图9;The change of nitrite content in sauce meat under different ultrasonic time conditions is shown in Figure 9;

由图9可知,对照1组的亚硝酸钠含量为0.143mg/kg,显著低于对照2组(P<0.05)。超声处理组肉样的亚硝酸钠含量显著低于两个对照组(P<0.05)。超声处理组中,随着超声时间的增大,肉样中的亚硝酸钠含量呈先降低后上升的趋势,以90min超声处理组肉样的亚硝酸钠含量最低(P<0.05)。It can be seen from Figure 9 that the sodium nitrite content in control group 1 was 0.143 mg/kg, which was significantly lower than that in control group 2 (P<0.05). The content of sodium nitrite in the ultrasonic treatment group was significantly lower than that in the two control groups (P<0.05). In the ultrasonic treatment group, as the ultrasonic time increased, the sodium nitrite content in the meat samples first decreased and then increased, and the sodium nitrite content in the 90-min ultrasonic treatment group was the lowest (P<0.05).

不同超声波时间条件下酱肉a*值的变化见图10;The change of the a* value of sauce meat under different ultrasonic time conditions is shown in Figure 10;

由图10可知,对照1组肉样的a*值稍低于对照2组,但差异不显著(P>0.05)。超声组肉样的a*值显著低于两个对照组(P<0.05)。超声处理组中,随着超声时间的增大,肉样中的a*值呈先降低后上升的趋势,以90min超声处理组肉样的a*值最低(P<0.05)。当超声时间增加到120min时,肉样的a*值变大,原因可能是超声时间过长,肉样中的细胞大量破裂,胞内色素释放,使a*值上升。It can be seen from Figure 10 that the a* value of meat samples in control group 1 was slightly lower than that in control group 2, but the difference was not significant (P>0.05). The a* value of the meat sample in the ultrasound group was significantly lower than that in the two control groups (P<0.05). In the ultrasonic treatment group, with the increase of ultrasonic time, the a* value in the meat samples first decreased and then increased, and the a* value of the meat samples in the 90-min ultrasonic treatment group was the lowest (P<0.05). When the ultrasonic time was increased to 120 minutes, the a* value of the meat sample became larger. The reason may be that the ultrasonic time was too long, a large number of cells in the meat sample ruptured, and the intracellular pigment was released, which increased the a* value.

不同超声波时间条件下酱肉的POV含量变化见图11;The changes of POV content of sauce meat under different ultrasonic time conditions are shown in Figure 11;

由图11可知,对照1组肉样的POV含量为0.07g/100g,显著低于对照2组(P<0.05)。超声处理组肉样的POV含量显著低于两个对照组(P<0.05)。超声处理组中,随着超声时间的延长,肉样的POV含量呈现先减少后增大的趋势,以90min超声组肉样的POV含量最低(P<0.05)。当超声时间增加到120min时POV含量有所上升,一方面原因是长时间超声处理会显著增加牛肉蛋白质氧化和脂肪氧化程度,加速蛋白质分解,促进脂肪分解和氧化;另一方面原因是超声波对食盐渗透有促进作用。当超声强度增强,食盐浓度增大,过氧化值也增大。It can be seen from Figure 11 that the POV content of meat samples in control group 1 was 0.07g/100g, which was significantly lower than that in control group 2 (P<0.05). The POV content of meat samples in the ultrasonic treatment group was significantly lower than that of the two control groups (P<0.05). In the ultrasonic treatment group, with the prolongation of ultrasonic time, the POV content of meat samples first decreased and then increased, and the POV content of meat samples in the 90-min ultrasonic group was the lowest (P<0.05). When the ultrasonic time increased to 120min, the POV content increased. On the one hand, the long-term ultrasonic treatment will significantly increase the oxidation of beef protein and fat, accelerate protein decomposition, and promote fat decomposition and oxidation; on the other hand, the reason is that ultrasonic treatment of salt Penetration is facilitated. When the ultrasonic intensity increases, the salt concentration increases, and the peroxide value also increases.

不同超声时间条件下酱肉的羰基价含量变化见图12;The change of carbonyl value content of sauce meat under different ultrasonic time conditions is shown in Figure 12;

由图12可知,对照2组肉样的羰基价稍高于对照1组,但差异不显著(P>0.05)。超声处理组肉样的羰基价显著低于两个对照组(P<0.05)。超声处理组中,随超声时间的延长,肉样的羰基价呈现先减少后增大的趋势,以90min超声组肉样的羰基价最低(P<0.05)。与图11趋势基本一致。It can be seen from Figure 12 that the carbonyl value of meat samples in control group 2 was slightly higher than that in control group 1, but the difference was not significant (P>0.05). The carbonyl value of meat samples in the ultrasonic treatment group was significantly lower than that of the two control groups (P<0.05). In the ultrasonic treatment group, with the prolongation of ultrasonic time, the carbonyl value of meat samples first decreased and then increased, and the carbonyl value of meat samples in the 90-min ultrasonic group was the lowest (P<0.05). It is basically consistent with the trend in Figure 11.

不同量香辛料提取液处理对酱肉中亚硝酸盐消除效果试验Experiment on the Elimination Effect of Different Amounts of Spice Extracts on the Elimination of Nitrite in Sauce Meat

以亚硝酸盐腌制的牛肉加工的酱肉为试验对象,将生姜、桂皮、八角复合提取液按肉与水总重的1%、2%、3%、4%、5%的量加入水中进行煮制牛肉,将处理好的原料肉分为7组。在超声功率为300W、时间为60min、频率为28kHz、温度为75℃的条件下煮制牛肉,以添加香辛料煮制而不经超声波处理的腌制肉样为对照组1,以清水煮制且不经超声波处理的肉样为对照组2,测定煮制前后肉样中亚硝酸盐的残留量及亚硝胺的含量等指标,试验不同量香辛料提取液对酱肉中残留亚硝酸盐消除效果及亚硝胺的阻断效率。Taking beef marinated with nitrite as the test object, the compound extracts of ginger, cinnamon and star anise were added to the water in the amount of 1%, 2%, 3%, 4%, and 5% of the total weight of the meat and water. The beef is boiled, and the processed raw meat is divided into 7 groups. The beef was boiled under the conditions of ultrasonic power of 300W, time of 60min, frequency of 28kHz, and temperature of 75°C. The marinated meat samples cooked with spices and not treated with ultrasonic were used as control group 1. The meat samples without ultrasonic treatment were used as the control group 2, the residual nitrite and nitrosamine content in the meat samples before and after cooking were measured, and the effects of different amounts of spice extracts on the elimination of residual nitrite in sauced meat were tested. and the blocking efficiency of nitrosamines.

不同香辛料提取液酱肉亚硝酸盐含量的变化见图13;The change of nitrite content in different spice extracts is shown in Figure 13;

由图13可知,对照1组肉样的亚硝酸钠含量为0.294mg/kg,显著低于对照2组(P<0.05)。超声处理组肉样的亚硝酸钠含量显著低于两个对照组(P<0.05)。超声处理组中,随香辛料提取液添加量增大,亚硝酸钠含量呈先降低后上升趋势,以2%添加量肉样中的亚硝酸钠含量最低(P<0.05)。当香辛料提取液超过3%时,肉样中的亚硝酸钠含量呈上升趋势,一方面可能是因为提取液中的天然色素对检测结果造成了影响;另一方面也可能是肉制品中存在的某些成分对香辛料的亚硝酸盐清除能力有一定的干扰作用,结果仍有待进一步试验。综合来看,添加量为2%的香辛料提取液清除肉样中亚硝酸盐的效果最好。It can be seen from Figure 13 that the sodium nitrite content of meat samples in control group 1 was 0.294 mg/kg, which was significantly lower than that in control group 2 (P<0.05). The content of sodium nitrite in the ultrasonic treatment group was significantly lower than that in the two control groups (P<0.05). In the ultrasonic treatment group, with the increase of spice extract, the content of sodium nitrite first decreased and then increased, and the content of sodium nitrite was the lowest in meat samples with 2% addition (P<0.05). When the spice extract exceeds 3%, the content of sodium nitrite in the meat sample is on the rise. On the one hand, it may be because the natural pigment in the extract has affected the test results; Some ingredients have a certain interference effect on the nitrite scavenging ability of spices, and the results still need further testing. On the whole, the addition of 2% spice extract has the best effect on removing nitrite in meat samples.

不同香辛料提取液处理酱肉中色差(a*值)的变化Changes of color difference (a* value) in sauce meat treated with different spice extracts

不同香辛料提取液酱肉a*值变化见图14;The change of a* value of sauce meat in different spice extracts is shown in Figure 14;

由图14可知,对照1组肉样的a*值稍低于对照2组,但差异不显著(P>0.05),原因可能是亚硝酸盐的发色作用主要在腌制过程发挥作用,当肉样煮制时,表面蛋白质变性,香辛料渗入较少,对肉样红度值影响不明显。处理组肉样的a*值显著低于两个对照组(P<0.05),原因是一定强度的超声处理,可提高肉的保水性,使肉样的红度值降低;另外还有可能是超声波处理加速了香辛料的渗入,香辛料自身的颜色影响了肉样的红度值。超声处理组中,随香辛料提取液的增大,a*值呈先减少后增加的趋势。2%处理组肉样的a*值显著低于1%处理组(P<0.05),原因可能是香辛料提取液添加量较少时,香辛料的抗氧化作用不明显,其自身的颜色影响了肉样的红度值。当香辛料提取液超过3%时,肉样的a*值呈上升趋势,原因可能是香辛料提取液在一定程度上促进了亚硝酸盐的发色。It can be seen from Figure 14 that the a* value of the meat samples in the control group 1 was slightly lower than that in the control group 2, but the difference was not significant (P>0.05). When the meat sample is cooked, the surface protein is denatured, and the spices penetrate less, which has little effect on the redness value of the meat sample. The a* value of the meat sample in the treatment group was significantly lower than that of the two control groups (P<0.05), because ultrasonic treatment of a certain intensity can improve the water retention of the meat and reduce the red value of the meat sample; Ultrasonic treatment accelerates the infiltration of spices, and the color of spices itself affects the redness value of meat samples. In the ultrasonic treatment group, with the increase of the spice extract, the a* value first decreased and then increased. The a* value of the meat sample in the 2% treatment group was significantly lower than that in the 1% treatment group (P<0.05). The reason may be that when the amount of spice extract was added less, the antioxidant effect of the spice was not obvious, and its own color affected the meat quality. Such redness value. When the spice extract exceeds 3%, the a* value of the meat sample tends to rise, the reason may be that the spice extract promotes the color development of nitrite to a certain extent.

不同香辛料提取液酱肉POV含量的变化见图15;The change of POV content of sauced meat in different spice extracts is shown in Figure 15;

由图15可知,对照1组肉样的POV含量为0.0913g/100g,显著低于对照2组(P<0.05)。处理组肉样的POV含量显著低于两个对照组(P<0.05)。处理组中,随香辛料提取液添加量增大,POV呈现先降低后上升趋势,以2%添加量肉样的POV含量最低(P<0.05)。当香辛料提取液超过3%时,肉样的POV含量呈上升趋势,原因可能是香辛料提取液与肉中的一些成分发生了反应,降低了香辛料的抗氧化作用;还有可能是在加热和超声条件下,香辛料提取液中某些成分发生了分解。综合考虑,2%香辛料提取液的氧化程度最小,效果最好。It can be seen from Figure 15 that the POV content of meat samples in control group 1 was 0.0913g/100g, which was significantly lower than that in control group 2 (P<0.05). The POV content of meat samples in the treatment group was significantly lower than that in the two control groups (P<0.05). In the treatment group, POV first decreased and then increased with the increase of spice extract, and the POV content of meat samples with 2% addition was the lowest (P<0.05). When the spice extract exceeds 3%, the POV content of the meat sample tends to rise. The reason may be that the spice extract reacts with some components in the meat, which reduces the antioxidant effect of the spice; Under certain conditions, some components in the spice extract were decomposed. Considering comprehensively, the oxidation degree of 2% spice extract is the least, and the effect is the best.

不同香辛料提取液酱肉羰基价含量的变化见图16;The change of the carbonyl value content of sauce meat in different spice extracts is shown in Figure 16;

由图16可知,对照1组肉样的羰基价稍低于对照2组,但差异不显著(P>0.05)。处理组肉样的羰基价显著低于两个对照组(P<0.05)。在处理组中,随香辛料提取液添加量增大,肉样的羰基价呈先降低后上升的趋势。2%添加量肉样的羰基价显著最低(P<0.05)。与图15趋势基本一致。It can be seen from Figure 16 that the carbonyl value of meat samples in control group 1 was slightly lower than that in control group 2, but the difference was not significant (P>0.05). The carbonyl value of meat samples in the treatment group was significantly lower than that in the two control groups (P<0.05). In the treatment group, the carbonyl value of the meat samples first decreased and then increased with the increase of spice extract addition. The carbonyl value of 2% added meat sample was significantly lowest (P<0.05). It is basically consistent with the trend in Figure 15.

不同超声条件和不同香辛料提取液条件下酱肉亚硝胺含量检测结果如下,根据国标GB5009.26-2016《食品中N-亚硝胺类化合物的测定》第一法气相色谱-质谱法并未检测出N-二甲基亚硝胺,具体结果见表3。The detection results of nitrosamine content in sauce meat under different ultrasonic conditions and different spice extracts are as follows. N-dimethylnitrosamine was detected, and the specific results are shown in Table 3.

表3酱肉中亚硝胺检测结果Table 3 Detection results of nitrosamines in sauce meat

由表4所见,由极差分析可知,超声频率、超声温度、超声时间、香辛料添加量对降低亚硝酸钠的含量的主次关系为:B>C>A>D,其中超声温度的影响最大,其次是超声时间,然后是超声频率,影响最小的是香辛料添加量。并得出最优配比为A3B2C3D1,即超声频率为40kHz、超声温度为80℃、超声时间100min、香辛料提取液添加量为1%时对于清除酱肉中残留的亚硝酸钠含量有着较好的效果,肉样中的亚硝酸盐含量降为0.0889mg/kg,与单独使用香辛料处理组相比,亚硝酸盐清除率达到了53.94%;与未经超声及香辛料处理组相比,亚硝酸盐清除率达到了47.41%。As can be seen from Table 4, it can be seen from the range analysis that the primary and secondary relationship of ultrasonic frequency, ultrasonic temperature, ultrasonic time, and spice addition to reducing the content of sodium nitrite is: B>C>A>D, wherein the influence of ultrasonic temperature The largest, followed by ultrasonic time, and then ultrasonic frequency, the least impact is the amount of spices added. And it is obtained that the optimal ratio is A3B2C3D1, that is, when the ultrasonic frequency is 40kHz, the ultrasonic temperature is 80°C, the ultrasonic time is 100min, and the amount of spice extract is 1%, it has a better effect on removing the residual sodium nitrite content in sauce meat. As a result, the nitrite content in the meat sample was reduced to 0.0889mg/kg, and compared with the group treated with spices alone, the nitrite removal rate reached 53.94%; compared with the group without ultrasound and spices, the nitrite The clearance rate reached 47.41%.

表4正交试验结果和极差分析Table 4 Orthogonal test results and range analysis

本试验的主要试验内容是通过设置不同的超声波频率、温度、时间和不同添加量的香辛料提取液(生姜、桂皮、八角三种复配),测量不同试验条件下酱肉的亚硝酸钠含量、色差、POV、羰基价等理化指标,试验超声波处理辅助香辛料对酱肉中残留亚硝酸盐含量的消除效果,为酱卤肉制品加工开发出一种亚硝酸盐清除技术,为低硝酱卤肉制品的生产提供一定的指导。试验结果如下:The main test content of this test is to measure the sodium nitrite content, Physical and chemical indicators such as color difference, POV, carbonyl value, etc., test the effect of ultrasonic treatment on the elimination of residual nitrite content in sauced meat with spices, and develop a nitrite removal technology for the processing of sauced meat products. The production of products provides certain guidance. The test results are as follows:

1.采用不同的超声波频率、温度、时间及不同香辛料添加量处理肉样,通过测定亚硝酸钠含量、色差、POV、羰基价等指标,试验了不同工艺条件及参数对肉样中亚硝酸盐的清除效果,结果发现超声频率为28kHz、超声温度为80℃、超声时间为90min及香辛料提取液添加量为2%时,对肉样中亚硝酸盐清除效果较适宜,且抗氧化效果较好。1. Treat meat samples with different ultrasonic frequencies, temperatures, times, and different spice additions. By measuring sodium nitrite content, color difference, POV, carbonyl value and other indicators, the effects of different process conditions and parameters on the nitrite in meat samples were tested. The results showed that when the ultrasonic frequency was 28kHz, the ultrasonic temperature was 80°C, the ultrasonic time was 90min, and the amount of spice extract was 2%, the removal effect of nitrite in meat samples was more suitable, and the anti-oxidation effect was better. .

2.根据单因素试验结果,选取超声频率(22kHz、28kHz、40kHz)、超声温度(75℃、80℃、85℃)、超声时间(80min、90min、100min),香辛料提取液添加量(1%、1.5%、2%)为试验因素,以肉样中亚硝酸盐含量为测定指标,进行了超声波处理辅助香辛料对酱肉中残留亚硝酸盐的消除效果工艺条件及参数的优化。结果表明:超声温度的影响最大,其次是超声时间,然后是超声频率,影响最小的是香辛料添加量,优化出最适工艺条件:超声频率为40kHz、超声温度为80℃、超声时间为100min、香辛料提取液添加量为1%时对于清除酱肉中残留的亚硝酸钠含量有着较好的效果。肉样中的亚硝酸盐含量降为0.0889mg/kg,与单独使用香辛料处理组相比,亚硝酸盐清除率达到了53.94%;与未经超声及香辛料处理组相比,亚硝酸盐清除率达到了47.41%。2. According to the single factor test results, select the ultrasonic frequency (22kHz, 28kHz, 40kHz), ultrasonic temperature (75°C, 80°C, 85°C), ultrasonic time (80min, 90min, 100min), and the amount of spice extract (1% , 1.5%, 2%) as the experimental factors, taking the content of nitrite in the meat sample as the measurement index, the process conditions and parameters of the elimination effect of ultrasonic treatment assisted spices on the residual nitrite in sauced meat were optimized. The results show that the ultrasonic temperature has the greatest impact, followed by the ultrasonic time, and then the ultrasonic frequency, and the least impact is the amount of spices added. The optimum process conditions are optimized: ultrasonic frequency is 40kHz, ultrasonic temperature is 80°C, ultrasonic time is 100min, When the spice extract is added at 1%, it has a good effect on removing the residual sodium nitrite content in sauced meat. The nitrite content in the meat sample was reduced to 0.0889mg/kg, compared with the group treated with spices alone, the nitrite removal rate reached 53.94%; compared with the group without ultrasound and spices treatment, the nitrite removal rate It reached 47.41%.

下面针对不同香辛料对亚硝酸盐的清除作用作出验证;The following is to verify the scavenging effect of different spices on nitrite;

材料与试剂,本试验所用材料与试剂见表5。Materials and reagents, the materials and reagents used in this test are listed in Table 5.

表5材料与试剂Table 5 Materials and Reagents

本试验所用主要仪器与设备见表6。The main instruments and equipment used in this test are listed in Table 6.

表6主要仪器与设备Table 6 Main instruments and equipment

试验方法experiment method

香辛料预处理:分别称取100g八角、桂皮、生姜三种香辛料,其中桂皮、八角用粉碎机粉碎至粉状,留取备用。生姜进行洗净、去皮、切碎等预处理,留取备用。Pretreatment of spices: Weigh 100g of star anise, cassia bark and ginger three spices respectively, wherein cinnamon bark and star anise are crushed to powder with a pulverizer, and set aside for later use. Ginger is washed, peeled, chopped and other pretreatments, and reserved for later use.

香辛料的提取及浓缩:分别采用水浸提、醇浸提、超声—水浸提法、超声—醇浸提法四种方法对八角、桂皮、生姜三种香辛料进行提取。Extraction and concentration of spices: four methods of water extraction, alcohol extraction, ultrasonic-water extraction, ultrasonic-alcohol extraction were used to extract three spices, star anise, cinnamon and ginger.

1.水浸提取:精确称取50.0g香辛料干粉(或切碎的生姜),放入250mL三角瓶中,加150mL蒸馏水振荡浸泡1h,温度为40℃,然后过滤,将滤液收集起来,用旋转蒸发仪浓缩至50mL于50mL容量瓶中(浓度为1g/ml)备用。1. Water immersion extraction: Accurately weigh 50.0g of spice dry powder (or chopped ginger), put it into a 250mL Erlenmeyer flask, add 150mL of distilled water, shake and soak for 1h at a temperature of 40°C, then filter, collect the filtrate, and spin Evaporator concentrated to 50mL in a 50mL volumetric flask (concentration 1g/ml) for later use.

2.醇浸提取:精确称取50.0g香辛料干粉(或切碎的生姜),放入250mL三角瓶中,加150mL无水乙醇振荡浸泡1h,温度为40℃,然后过滤,将滤液收集起来,用旋转蒸发仪浓缩至50mL于50mL容量瓶中(浓度为1g/ml)备用。2. Alcoholic extraction: Accurately weigh 50.0g of dry spice powder (or chopped ginger), put it into a 250mL Erlenmeyer flask, add 150mL of absolute ethanol and shake and soak for 1h at a temperature of 40°C, then filter and collect the filtrate. Concentrate to 50mL with a rotary evaporator and store in a 50mL volumetric flask (concentration is 1g/ml) for later use.

3.超声—水浸提取法:精确称取50.0g香辛料粉(或切碎的生姜),放入250mL三角瓶中加150mL蒸馏水振荡浸泡1h,温度为40℃,放入超声波细胞粉碎机中,在25KHz、300W下提取25min,然后过滤,将滤液收集起来,用旋转蒸发仪浓缩至50mL于50mL容量瓶中(浓度为1g/ml)备用。3. Ultrasonic-water immersion extraction method: Accurately weigh 50.0g of spice powder (or chopped ginger), put it into a 250mL Erlenmeyer flask, add 150mL of distilled water and shake and soak for 1h at a temperature of 40°C, put it into an ultrasonic cell pulverizer, Extract at 25KHz, 300W for 25min, then filter, collect the filtrate, concentrate to 50mL with a rotary evaporator and put it in a 50mL volumetric flask (concentration is 1g/ml) for later use.

4.超声—醇浸提取法:精确称取50.0g香辛料粉(或切碎的生姜),放入250mL三角瓶中加150mL无水乙乙醇振荡浸泡1h,温度为40℃,放入超声波细胞粉碎机中,在25KHz、300W下提取25min,然后过滤,将滤液收集起来,用旋转蒸发仪浓缩至50mL于50mL容量瓶中(浓度为1g/ml)备用。4. Ultrasonic-alcoholic extraction method: Accurately weigh 50.0g of spice powder (or chopped ginger), put it into a 250mL Erlenmeyer flask, add 150mL of anhydrous ethanol, shake and soak for 1h at a temperature of 40°C, put it into an ultrasonic cell crush In the machine, extract at 25KHz, 300W for 25min, then filter, collect the filtrate, concentrate to 50mL with a rotary evaporator and put it in a 50mL volumetric flask (concentration is 1g/ml) for subsequent use.

吸取提取液(浓度为1g/mL)1mL分别置于50mL具塞试管中,加水至刻度,混匀。对其进行亚硝酸盐的清除率的测定,根据清除效果的差异,分别选择出八角、桂皮、生姜各自的最佳提取方法。Draw 1mL of the extract (concentration: 1g/mL) into 50mL stoppered test tubes, add water to the mark, and mix well. The scavenging rate of nitrite was measured, and according to the differences in scavenging effects, the best extraction methods for star anise, cassia bark and ginger were selected respectively.

吸取各香辛料的最佳提取方法得到的提取液(浓度为1g/mL)1mL、2mL、3mL、4mL,分别置于50mL具塞试管中,加水至刻度,混匀。对其进行亚硝酸盐的清除率的测定,根据清除效果的差异研究香辛料提取液不同添加量对亚硝酸盐清除的影响。Take 1mL, 2mL, 3mL, and 4mL of the extracts (concentration: 1g/mL) obtained by the best extraction method for each spice, put them in 50mL stoppered test tubes, add water to the mark, and mix well. The scavenging rate of nitrite was measured, and the effect of different additions of spice extracts on scavenging nitrite was studied according to the difference in scavenging effect.

吸取各香辛料的最佳提取方法提取得到的提取液(浓度为1g/mL),选八角提取液量0.5mL、1mL、2mL,桂皮提取液量2mL、3mL、4mL,生姜提取液量2mL、3mL、4mL。按因素水平安排表(表7)进行复配,分别置于50mL具塞试管中,加水至刻度,混匀,进行三种香辛料复配的正交试验,以亚硝酸盐清除率为测定指标,优化出八角、桂皮、生姜对亚硝酸盐清除的最适配比。Absorb the best extraction method of each spice to extract the extract (concentration is 1g/mL), choose star anise extract volume 0.5mL, 1mL, 2mL, cassia bark extract volume 2mL, 3mL, 4mL, ginger extract volume 2mL, 3mL , 4mL. Carry out compound according to factor level arrangement table (table 7), be placed in 50mL test tube with stopper respectively, add water to scale, mix, carry out the orthogonal experiment of three kinds of spices compound, measure index with nitrite scavenging rate, Optimize the optimum ratio of star anise, cinnamon and ginger to nitrite removal.

表7正交试验因素水平安排表Table 7 Orthogonal test factor level arrangement table

亚硝酸盐清除率的测定:分别取各种提取液10mL于50mL容量瓶中,然后再加入配制好的25mLpH为3.0的柠檬酸钠-盐酸缓冲溶液,再加入100mg/kg的NaNO2溶液5mL,最后用蒸馏水定容至刻度,并在恒温箱内,37℃恒温1h。然后用移液枪各吸取1mL反应液于25mL具塞试管内,再分别加入质量分数为2mL4g/L的对氨基苯磺酸溶液,混匀,静置3min~5min后各加入质量分数为2mL2g/L盐酸萘乙二胺溶液,加水至刻度,混匀,静置15min。用分光光度计在540nm处测吸光度,分别用相应浓度相同用量的提取液做空白试验,最后下式亚硝酸盐计算清除率。Determination of nitrite scavenging rate: Take 10mL of various extracts in a 50mL volumetric flask, then add 25mL of sodium citrate-hydrochloric acid buffer solution with a pH of 3.0, and then add 5mL of 100mg/kg NaNO2 solution, Finally, the volume was adjusted to the mark with distilled water, and the temperature was kept at 37°C for 1 hour in a constant temperature box. Then use a pipette gun to draw 1mL of the reaction solution into 25mL test tubes with stoppers, and then add 2mL4g/L p-aminobenzenesulfonic acid solution respectively, mix well, let stand for 3min to 5min, and then add 2mL2g/L p-aminobenzenesulfonic acid solution respectively. L naphthaleneethylenediamine hydrochloride solution, add water to the mark, mix well, let stand for 15min. Use a spectrophotometer to measure the absorbance at 540nm, respectively use the same concentration and the same amount of extract as a blank test, and finally calculate the clearance rate of nitrite with the following formula.

清除率=(A0-Ax)/A0×100%Clearance rate = (A 0 -A x )/A 0 ×100%

式中:A0-加入相应提取液空白试验的吸光度;In the formula: A 0 - the absorbance of the blank test with the corresponding extract;

Ax-加入不同浓度提取液时的吸光度。A x - Absorbance when different concentrations of extracts are added.

每个实验进行3次平行试验,结果表示为平均数。实验图表采用SigmaPlot12.5绘制,利用SPSS17.0进行显著性分析,显著性水平0.05。Three parallel experiments were carried out for each experiment, and the results were expressed as the average. The experimental charts were drawn using SigmaPlot12.5, and SPSS17.0 was used for significance analysis with a significance level of 0.05.

香辛料各自最适提取方法的筛选:由图17可见,针对八角提取物对亚硝酸盐清除率来讲,醇提法、超声-醇提法、超声-水提法显著优于水提法(P<0.05),而超声与醇协助效果无差异,超声与水协助效果明显。原因可能是八角中存在对亚硝酸盐有清除作用的某些物质与水相比更容易溶于无水乙醇中,提取效率比较好,超声波作用不明显,水提取时的提取效率不是太好,使用超声就可以提高其提取效率。针对桂皮提取物对亚硝酸盐清除率来讲,醇提法明显优于水提取法、超声-水提取法(P<0.05),略高于超声-醇提取法(P>0.05),使用超声协助效果变差。其原因可能由于桂皮中存在的对亚硝酸盐清除物质,与水相比更容易溶于无水乙醇中。使用超声波辅助会对这种物质具有破坏作用,降低其清除作用。针对生姜提取物对亚硝酸盐清除率来讲,以醇提取时,其提取效果几乎没有,甚至会小于空白对照组,明显小于水提取(P<0.05)。其原因可能是醇会破坏生姜中有效成分,使用超声协助也会破坏有效成分。在四种提取方法中,八角、桂皮以醇提取法效果较好,生姜以水提取法效果较好。Screening of the respective optimal extraction methods of spices: As seen from Figure 17, for the nitrite scavenging rate of star anise extract, alcohol extraction, ultrasonic-alcohol extraction, ultrasonic-water extraction are significantly better than water extraction (P <0.05), while there was no difference in the effect of ultrasound and alcohol assistance, but the effect of ultrasound and water assistance was obvious. The reason may be that there are certain substances in star anise that have a scavenging effect on nitrite, which are easier to dissolve in absolute ethanol than water, and the extraction efficiency is better. The ultrasonic effect is not obvious, and the extraction efficiency during water extraction is not very good. The extraction efficiency can be improved by using ultrasound. Regarding the removal rate of cinnamon bark extract on nitrite, the alcohol extraction method is significantly better than the water extraction method and ultrasonic-water extraction method (P<0.05), slightly higher than the ultrasonic-alcohol extraction method (P>0.05). Assistance becomes less effective. The reason for this may be due to the presence of nitrite scavenging substances in cinnamon bark, which are more soluble in absolute ethanol than water. The use of ultrasonic assistance can have a damaging effect on this substance, reducing its removal. Regarding the nitrite scavenging rate of ginger extract, when extracted with alcohol, its extraction effect is almost insignificant, even lower than that of the blank control group, and significantly lower than that of water extraction (P<0.05). The reason may be that alcohol will destroy the active ingredients in ginger, and the use of ultrasonic assistance will also destroy the active ingredients. Among the four extraction methods, alcohol extraction for star anise and cinnamon bark is better, and water extraction for ginger is better.

三种香辛料提取液的不同添加量对亚硝酸盐清除效果的单因素试验:由图18可见,在提取液添加量为1mL的浓度下,桂皮对亚硝酸盐的清除效果达到65%,八角达到52%,生姜只有6.18%。随着浓度的增加,桂皮、生姜的清除效果上升,桂皮的清除效果上升明显(P<0.05),生姜清除效果上升不显著(P>0.05)。随着浓度的增加,八角的清除效果不断下降。由此选定桂皮提取液添加量为4mL,八角提取液添加量为1mL,生姜提取液添加量为4mL。The single factor test of the different additions of three kinds of spice extracts on the scavenging effect of nitrite: As can be seen from Figure 18, at the concentration of 1 mL of the extract, the scavenging effect of cassia bark to nitrite reaches 65%, and star anise reaches 65%. 52%, ginger only 6.18%. With the increase of the concentration, the scavenging effect of cinnamon and ginger increased, the scavenging effect of cinnamon increased significantly (P<0.05), and the scavenging effect of ginger did not increase significantly (P>0.05). As the concentration increased, the scavenging effect of star anise decreased continuously. Therefore, the selected cassia bark extract addition amount is 4mL, the star anise extract addition amount is 1mL, and the ginger extract addition amount is 4mL.

三种香辛料对亚硝酸盐清除的正交试验:由表8所见,由极差分析可知,八角、桂皮、生姜对亚硝酸盐清除率影响的主次关系为:A>B>C,其中八角的影响最大,桂皮次之,影响最小的为生姜。并得出最优配比为A3B1C3,即八角:桂皮:生姜八角为1:1:2时对于亚硝酸盐的清除有着较好的效果。Orthogonal test of three kinds of spices on nitrite scavenging: As can be seen from Table 8, it can be seen from the range analysis that the primary and secondary relationship of star anise, cinnamon, and ginger on the nitrite scavenging rate is: A>B>C, where Star anise had the greatest impact, followed by cinnamon, and ginger had the least impact. And it is concluded that the optimal ratio is A3B1C3, that is, star anise: cinnamon bark: ginger star anise is 1:1:2, which has a better effect on the removal of nitrite.

表8正交试验结果及极差分析Table 8 Orthogonal test results and range analysis

本试验结果表明八角、桂皮的最适提取方法为醇提取法,而生姜的最适提取方法为水提取法。通过单因素试验选定桂皮提取液添加量为4mL,八角提取液添加量为1mL,生姜提取液添加量为4mL。经过正交试验优化得到三种香辛料最适配比,即八角:桂皮:生姜八角为1:1:2时对于亚硝酸盐的清除效果最优。The results of this experiment show that the optimum extraction method of star anise and cassia bark is alcohol extraction, while the optimum extraction method of ginger is water extraction. Through the single factor test, the addition amount of cassia bark extract is 4mL, the addition amount of star anise extract is 1mL, and the addition amount of ginger extract is 4mL. The most suitable ratio of three kinds of spices was obtained through the optimization of orthogonal experiment, that is, star anise: cinnamon bark: ginger star anise was 1:1:2, which had the best scavenging effect on nitrite.

Claims (5)

1. a kind of method for reducing sauce Nitrite Content of meat products determined, it is characterised in that: the following steps are included:
S1, beef is pickled, salt down to beef is in butcher's meat color or kermesinus to color completely, is terminated marinated;
S2, the beef pickled is put into container, water is added in a reservoir and composite aromatic condiment extracting solution, composite aromatic condiment mention The weight of liquid is taken to account for the 1%~5% of beef and water total weight;
S3, the beef in container is cooked, while ultrasonic response is carried out to beef using supersonic generator, it will be ultrasonic The tranmitting frequency of wave is set as 22kHz~40kHz, the reaction temperature of ultrasonic wave is set as to 75 DEG C~85 DEG C;
S4, after cooking 60min~120min, supersonic generator is closed, beef is pulled out, is cooled to room temperature.
2. reducing the method for sauce Nitrite Content of meat products determined as described in claim 1, it is characterised in that: the step S2 The preparation of middle composite aromatic condiment extracting solution the following steps are included:
S21, three kinds of illiciumverum, cassia bark, ginger spices are weighed respectively, cassia bark, illiciumverum are crushed to powdery with pulverizer, by ginger It cleans, peeling, chopping, it is spare;
S22, octagonal, cassia bark is extracted respectively using alcohol leaching extraction method;It is put into octagonal or cassia bark powder in a reservoir, is added 75% ethyl alcohol of 3 times of volumes, 1h is impregnated in oscillation at 40 DEG C, then filters, filtrate is collected, with Rotary Evaporators at 50 DEG C At a temperature of be concentrated, respectively obtain octagonal concentrate and cassia bark concentrate;
S23, ginger is extracted using water logging extraction method;It is put into the ginger of chopping in a reservoir, adds the distillation of 3 times of volumes Water, 1h is impregnated in oscillation at 40 DEG C, then filters, filtrate is collected, be concentrated at a temperature of 64 DEG C with Rotary Evaporators, Obtain ginger concentrate;
S24, octagonal concentrate, cassia bark concentrate, ginger concentrate are mixed in the ratio of 1:1:2, obtains composite pungent and fragrant Expect extracting solution.
3. reducing the method for sauce Nitrite Content of meat products determined as described in claim 1, it is characterised in that: the step S2 The weight of middle composite aromatic condiment extracting solution accounts for the 1% of beef and water total weight.
4. reducing the method for sauce Nitrite Content of meat products determined as claimed in claim 3, it is characterised in that: the step S3 The tranmitting frequency of middle ultrasonic wave is set as 40kHz, the reaction temperature of ultrasonic wave is set as 80 DEG C.
5. reducing the method for sauce Nitrite Content of meat products determined as claimed in claim 4, it is characterised in that: the step S4 Middle brew time is set as 100min.
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