CN105115965A - Soft drink synthetic pigment fast detection method and kit - Google Patents
Soft drink synthetic pigment fast detection method and kit Download PDFInfo
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- CN105115965A CN105115965A CN201510447152.0A CN201510447152A CN105115965A CN 105115965 A CN105115965 A CN 105115965A CN 201510447152 A CN201510447152 A CN 201510447152A CN 105115965 A CN105115965 A CN 105115965A
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- 239000001040 synthetic pigment Substances 0.000 title claims abstract description 43
- 238000001514 detection method Methods 0.000 title claims abstract description 41
- 235000014214 soft drink Nutrition 0.000 title claims description 19
- 239000000049 pigment Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002585 base Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000004952 Polyamide Substances 0.000 claims description 13
- 229920002647 polyamide Polymers 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000007790 solid phase Substances 0.000 claims description 9
- 235000012730 carminic acid Nutrition 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 229920002292 Nylon 6 Polymers 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 235000012756 tartrazine Nutrition 0.000 claims description 5
- 239000004149 tartrazine Substances 0.000 claims description 5
- UJMBCXLDXJUMFB-GLCFPVLVSA-K tartrazine Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-GLCFPVLVSA-K 0.000 claims description 5
- 229960000943 tartrazine Drugs 0.000 claims description 5
- 240000001592 Amaranthus caudatus Species 0.000 claims description 4
- 235000009328 Amaranthus caudatus Nutrition 0.000 claims description 4
- 235000012735 amaranth Nutrition 0.000 claims description 4
- 239000004178 amaranth Substances 0.000 claims description 4
- IINNWAYUJNWZRM-UHFFFAOYSA-L erythrosin B Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(I)C(=O)C(I)=C2OC2=C(I)C([O-])=C(I)C=C21 IINNWAYUJNWZRM-UHFFFAOYSA-L 0.000 claims description 4
- 235000012732 erythrosine Nutrition 0.000 claims description 4
- 239000004174 erythrosine Substances 0.000 claims description 4
- 229940011411 erythrosine Drugs 0.000 claims description 4
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- OIQPTROHQCGFEF-UHFFFAOYSA-L chembl1371409 Chemical compound [Na+].[Na+].OC1=CC=C2C=C(S([O-])(=O)=O)C=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 OIQPTROHQCGFEF-UHFFFAOYSA-L 0.000 claims description 3
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000003463 adsorbent Substances 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 235000005979 Citrus limon Nutrition 0.000 description 3
- 244000131522 Citrus pyriformis Species 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 3
- 238000004040 coloring Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 235000015203 fruit juice Nutrition 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- -1 new red Chemical compound 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000004809 thin layer chromatography Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
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- 235000012741 allura red AC Nutrition 0.000 description 1
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- 201000011510 cancer Diseases 0.000 description 1
- CEZCCHQBSQPRMU-UHFFFAOYSA-L chembl174821 Chemical compound [Na+].[Na+].COC1=CC(S([O-])(=O)=O)=C(C)C=C1N=NC1=C(O)C=CC2=CC(S([O-])(=O)=O)=CC=C12 CEZCCHQBSQPRMU-UHFFFAOYSA-L 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
本发明公开了一种合成色素快速检测方法及其检测试剂盒的制备方法，调节样品酸碱度，将速测卡放入样品中，振摇5分钟，使速测卡与样品中的合成色素充分结合，取出速测卡，自然晾干，观察速测卡的颜色，可以判断样品中是否含有合成色素，以及含量范围。色素检测卡上含有吸附剂，卡片有多个规格，可依据样品中色素的含量选择相应规格的检测卡。本发明公开的检测方法不需要复杂的检测设备和仪器，操作简便、成本低、检测时间短，检测灵敏度较好，结果准确，可用于现场快速检测和样品筛查。本方法无毒无害，不会对环境造成危害。The invention discloses a rapid detection method for synthetic pigments and a preparation method of the detection kit. The acid-base value of the sample is adjusted, and the quick test card is put into the sample, and shaken for 5 minutes, so that the quick test card is fully combined with the synthetic pigment in the sample. , Take out the quick test card, let it dry naturally, observe the color of the quick test card, you can judge whether the sample contains synthetic pigments, and the content range. The pigment test card contains an adsorbent, and the card has multiple specifications, and the test card of the corresponding specification can be selected according to the content of the pigment in the sample. The detection method disclosed by the invention does not require complex detection equipment and instruments, has the advantages of simple operation, low cost, short detection time, good detection sensitivity and accurate results, and can be used for on-site rapid detection and sample screening. The method is non-toxic and harmless, and will not cause harm to the environment.
Description
技术领域technical field
本发明涉及软饮料中合成色素快速检测的方法及速测盒。The invention relates to a method for rapid detection of synthetic pigments in soft drinks and a rapid detection box.
背景技术Background technique
合成色素具有物理性质稳定，价格低廉，易着色而广受食品生产厂家的青睐，在软饮料中大量使用合成色素已经成为一种常态，市场上许多不法商家将其滥用于食品等违法行为，或谎称是天然色素。软饮料中的合成色素主要有苋菜红、胭脂红、柠檬黄、新红、赤藓红、诱惑红、日落黄等。这些合成色素长期低剂量摄入，存在致癌、致畸、致突变的可能性，须严格控制其在软饮料中的使用。目前检测这些合成色素的方法是：纸层析法、分光光度法、高效液相色谱法、薄层色谱法、示波极谱法等。Synthetic pigments have stable physical properties, low price, and easy coloring, so they are widely favored by food manufacturers. It has become a norm to use a large amount of synthetic pigments in soft drinks. Called natural pigment. Synthetic pigments in soft drinks mainly include amaranth, carmine, tartrazine, new red, erythrosine, allura red, sunset yellow, etc. Long-term low-dose intake of these synthetic pigments may cause cancer, teratogenicity, and mutagenesis, and their use in soft drinks must be strictly controlled. The current methods for detecting these synthetic pigments are: paper chromatography, spectrophotometry, high performance liquid chromatography, thin layer chromatography, oscillographic polarography, etc.
这些方法检测准确，但检测时间长，过程复杂，且需要专业技术人员参与，价格昂贵，不便于现场检测。These methods are accurate in detection, but the detection time is long, the process is complicated, and professional and technical personnel are required to participate, the price is expensive, and it is not convenient for on-site detection.
发明内容Contents of the invention
为了解决背景技术中所述的对食品中合成色素检测传统方法所存在的问题，本发明设计一种快速检测方法和速测盒，达到操作简便，高灵敏，低成本，安全环保，用于对软饮料中合成色素进行快速定性及定量检测。In order to solve the problems existing in the traditional method for detecting synthetic pigments in food described in the background technology, the present invention designs a rapid detection method and a rapid detection box to achieve simple operation, high sensitivity, low cost, safety and environmental protection, and is used for the detection of Rapid qualitative and quantitative detection of synthetic pigments in soft drinks.
本发明采用的技术方案如下：The technical scheme that the present invention adopts is as follows:
软饮料中合成色素快速检测方法，用酸碱调节剂调节待测样品pH值至3-5后，将色素速测卡置于待测样品中，充分振摇反应5-10min后，取出色素速测卡，室温下自然晾干，观察色素速测卡的颜色，根据颜色变化，判断样品中是否含有合成色素；所述色素速测卡由耐酸碱的固相基体和喷涂在固相基体上的聚酰胺材料构成。Rapid detection method of synthetic pigments in soft drinks. After adjusting the pH value of the sample to be tested to 3-5 with an acid-base regulator, place the pigment quick test card in the sample to be tested, shake it fully for 5-10 minutes, and then take out the pigment for quick test. Card, dry naturally at room temperature, observe the color of the pigment quick test card, and judge whether the sample contains synthetic pigment according to the color change; the pigment quick test card is composed of an acid and alkali resistant solid phase Polyamide material composition.
所述合成色素为新红、苋菜红、赤藓红、胭脂红、柠檬黄、日落黄、或亮蓝。The synthetic pigment is new red, amaranth, erythrosine, carmine, tartrazine, sunset yellow, or brilliant blue.
为了达到更好的技术效果：In order to achieve a better technical effect:
将色素速测卡与标准比色卡进行颜色比对，可对样品中合成色素的含量进行半定量测定。Comparing the color of the quick test card with the standard color comparison card, the content of synthetic pigments in the sample can be semi-quantitatively determined.
所述的酸碱调节剂，包含了酸性调节剂和碱性调节剂两种。所述酸碱调节剂：酸碱调节剂为0.2-0.5g/ml柠檬酸溶液，碱性调节剂为浓度0.2-0.5g/ml氢氧化钠溶液；The acid-base regulator includes two kinds of acid regulator and alkaline regulator. The acid-base regulator: the acid-base regulator is 0.2-0.5g/ml citric acid solution, and the alkaline regulator is 0.2-0.5g/ml sodium hydroxide solution;
喷涂的聚酰胺厚度为0.05-0.1mm，聚酰胺材料为尼龙6或尼龙66，优选地选择尼龙6。软饮料中合成色素快速检测试剂盒，由酸碱调节剂、色素速测卡和标准比色卡组成：The thickness of the sprayed polyamide is 0.05-0.1 mm, and the polyamide material is nylon 6 or nylon 66, preferably nylon 6. Synthetic pigment rapid detection kit in soft drinks, composed of acid-base regulator, pigment rapid test card and standard color comparison card:
所述酸碱调节剂：酸碱调节剂为0.2-0.5g/ml柠檬酸溶液；碱性调节剂为浓度0.2-0.5g/ml氢氧化钠溶液；The acid-base regulator: the acid-base regulator is 0.2-0.5g/ml citric acid solution; the alkaline regulator is 0.2-0.5g/ml sodium hydroxide solution;
所述色素速测卡：由耐酸碱的固相基体和喷涂在固相基体上的聚酰胺构成，优选地聚酰胺膜厚度为0.05-0.1mm；The pigment quick test card: it is composed of an acid and alkali resistant solid phase substrate and polyamide sprayed on the solid phase substrate, preferably the thickness of the polyamide film is 0.05-0.1mm;
所述标准比色卡：配制含标准浓度合成色素水溶液，用酸碱调节剂调节pH值至3-5，将色素速测卡置于其中，充分振摇反应5-10min后，取出色素速测卡，室温下自然晾干，即得该标准浓度合成色素的标准比色卡。以此可以制出不同标准浓度合成色素的标准比色卡。The standard color comparison card: prepare an aqueous solution containing a synthetic pigment with a standard concentration, adjust the pH value to 3-5 with an acid-base regulator, place the pigment quick test card in it, shake it fully for 5-10 minutes, and then take out the pigment quick test card, and let it dry naturally at room temperature to get the standard color card of the standard concentration synthetic pigment. In this way, standard color cards of synthetic pigments with different standard concentrations can be produced.
通过聚酰胺材料对合成色素吸附，然后洗去杂质，再对结果进行判别。The synthetic pigment is adsorbed by the polyamide material, and then the impurities are washed away, and then the result is judged.
为了保持速测卡的稳定性和防止潮湿，最好采用单个密封包装。In order to maintain the stability of the rapid test card and protect it from moisture, it is best to use individual airtight packaging.
为了方便测定时振摇，色素速测卡上还有把手，最好是塑料把手。In order to facilitate the shaking during the determination, there is a handle on the pigment quick test card, preferably a plastic handle.
本发明的有益效果：Beneficial effects of the present invention:
本产品是对软饮料中合成色素的快速检测方法。使用本产品检测软饮料中的合成色素，无须另外配制试剂，操作简便，不需要专业人员即可进行。速测盒中不含有有毒有害腐蚀刺激性药品，不会对环境造成危害。本产品检测时间在10min以内，检测时间短，特异性强，结果易于判断，适合于现场快速检测和基层工作。This product is a rapid detection method for synthetic colorants in soft drinks. Using this product to detect synthetic pigments in soft drinks does not require additional preparation of reagents, and is easy to operate without the need for professionals. The quick test box does not contain toxic, harmful, corrosive and irritating drugs, and will not cause harm to the environment. The detection time of this product is within 10 minutes, the detection time is short, the specificity is strong, the result is easy to judge, and it is suitable for on-site rapid detection and grassroots work.
附图说明Description of drawings
图1是标准比色卡示例图Figure 1 is an example of a standard color card
具体实施方式Detailed ways
实施例1色素速测卡Embodiment 1 Pigment Quick Test Card
软饮料中合成色素快速检测试剂盒由酸碱调节剂、色素速测卡和标准比色卡组成；The rapid detection kit for synthetic pigments in soft drinks consists of an acid-base regulator, a rapid pigment test card and a standard color comparison card;
色素速测卡的固相基材是由耐酸碱的合成塑料制成的正圆形卡片，直径10mm。固相基材上喷涂聚酰胺材料(尼龙6)，厚度为0.1mm；色素速测卡上还有把手；The solid phase substrate of the pigment quick test card is a round card made of acid and alkali resistant synthetic plastic, with a diameter of 10mm. Polyamide material (nylon 6) is sprayed on the solid phase substrate with a thickness of 0.1mm; there is also a handle on the pigment quick test card;
其中酸碱调节剂：酸碱调节剂为0.2-0.5g/ml柠檬酸溶液，碱性调节剂为浓度0.2-0.5g/ml氢氧化钠溶液；Wherein the acid-base regulator: the acid-base regulator is 0.2-0.5g/ml citric acid solution, and the alkaline regulator is 0.2-0.5g/ml sodium hydroxide solution;
标准比色卡：配制含标准浓度合成色素水溶液，用酸碱调节剂调节pH值至3-5，将色素速测卡置于其中，充分振摇反应(或涡旋振荡)5-10min后，取出色素速测卡，室温下自然晾干，即得该标准浓度合成色素的标准比色卡。图1为几种色素的标准比色卡。Standard color comparison card: Prepare an aqueous solution containing a standard concentration of synthetic pigment, adjust the pH value to 3-5 with an acid-base regulator, place the color quick test card in it, fully shake the reaction (or vortex) for 5-10 minutes, then Take out the quick test card of the pigment, let it dry naturally at room temperature, and obtain the standard color comparison card of the synthetic pigment of the standard concentration. Figure 1 is a standard color card for several pigments.
检测：Detection:
将果汁轻轻摇匀，取20ml置于样品管中。用酸碱调节剂调节待测样品pH值至3-5。取色素速测卡浸入到样品中，振摇5～8分钟后取出用纯净水喷洗卡片。自然条件下晾干，若速测卡有颜色，说明果汁样品含有合成色素如新红、苋菜红、赤藓红、胭脂红、柠檬黄、日落黄、或亮蓝；若无颜色，说明样品不含合成色素。根据色素速测卡的颜色，与标准比色卡进行比色，可判读果汁样品中合成色素的含量。Shake the juice gently, take 20ml and put it in the sample tube. Adjust the pH value of the sample to be tested to 3-5 with an acid-base regulator. Take the pigment quick test card and dip it into the sample, shake it for 5-8 minutes, take it out and spray the card with pure water. Dry under natural conditions, if the quick test card has color, it means that the juice sample contains synthetic pigments such as new red, amaranth, erythrosine, carmine, lemon yellow, sunset yellow, or bright blue; if there is no color, it means that the sample is not Contains synthetic colourings. According to the color of the pigment quick test card, the color comparison with the standard color comparison card can be used to judge the content of the synthetic pigment in the juice sample.
实施例2：速测卡检测方式比较Example 2: Comparison of the detection methods of the quick test card
比较速测卡检测方式(振摇与不振摇)对于色素吸附效果的影响。Compare the effect of quick test card detection method (shaking and non-shaking) on the pigment adsorption effect.
分别配制1.0mg/L的柠檬黄、日落黄和胭脂红三种色素标准品溶液。分别取20ml置于样品管中(每种色素标准品分别取2管)，用酸碱调节剂调节pH值至3-5。将色素速测卡放入样品管，每种色素标准品的其中一管充分振摇5-10min，另一管不振摇，取出速测卡用纯净水喷洗卡片，自然条件下晾干。结果表明，振摇检测方式明显优于不振摇(表1)。Prepare 1.0 mg/L standard solutions of tartrazine, sunset yellow and carmine respectively. Take 20ml and place them in sample tubes (take 2 tubes for each color standard), and adjust the pH value to 3-5 with an acid-base regulator. Put the quick test card into the sample tube, fully shake one tube of each color standard product for 5-10 minutes, and not shake the other tube, take out the quick test card, spray the card with pure water, and dry it under natural conditions. The results showed that the shake detection method was significantly better than no shake (Table 1).
有振摇和无振摇的检测结果Test results with and without shaking
注：“-”表示未检出，“+”表示检出，“+”越多表示相对于只有一个时的颜色更加明显。Note: "-" means not detected, "+" means detected, and the more "+" means the color is more obvious than when there is only one.
实施例:3：速测卡方法与国家标准方法(薄层色谱法和高效液相色谱法)的比较Embodiment: 3: the comparison of quick test card method and national standard method (thin layer chromatography and high performance liquid chromatography)
采集市售10种不同品牌的果汁，分别采用本发明所述方法(实施例1)和国家标准GB/T5009.35-2003所述方法进行检测。结果如表2所示，本发明所述方法的结果与国家标准方法的检测结果一致。10 commercially available fruit juices of different brands were collected and detected by the method described in the present invention (Example 1) and the method described in the national standard GB/T5009.35-2003 respectively. The results are shown in Table 2, and the results of the method of the present invention are consistent with the detection results of the national standard method.
表2市售果汁检测结果比较Table 2 Comparison of test results of commercially available fruit juices
注：“-”表示未检出，“+”表示检出。Note: "-" means not detected, "+" means detected.
实施例4：三种合成色素速测卡法最低检测限的确定Embodiment 4: Determination of the minimum detection limit of three kinds of synthetic pigment rapid test cards
分别配制浓度为0.1mg/L,0.2mg/L,0.3mg/L,0.4mg/L,0.5mg/L,1.0mg/L,2.0mg/L,3.0mg/L,4.0mg/L的柠檬黄、日落黄和胭脂红三种色素标准品溶液。用按照实施例2中振摇方式进行检测，根据显色卡的颜色，得到柠檬黄、日落黄和胭脂红的最低检测限为0.3mg/L，0.4mg/L，0.4mg/L，远低于国家标准GB2760-2011规定的三种合成色素最大添加量：柠檬黄0.1g/kg、日落黄0.1g/kg、胭脂红0.05g/kg。Prepare lemons with concentrations of 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L Yellow, sunset yellow and carmine three pigment standard solutions. Detect with the shaking method in Example 2, according to the color of the color card, the minimum detection limit of tartrazine, sunset yellow and carmine is 0.3mg/L, 0.4mg/L, 0.4mg/L, far lower The maximum amount of three synthetic pigments specified in the national standard GB2760-2011: lemon yellow 0.1g/kg, sunset yellow 0.1g/kg, carmine 0.05g/kg.
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