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CN108627583A - The detection method of royal jelly ingredient the amount of migration in a kind of filter stick - Google Patents

The detection method of royal jelly ingredient the amount of migration in a kind of filter stick Download PDF

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Publication number
CN108627583A
CN108627583A CN201810467705.2A CN201810467705A CN108627583A CN 108627583 A CN108627583 A CN 108627583A CN 201810467705 A CN201810467705 A CN 201810467705A CN 108627583 A CN108627583 A CN 108627583A
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heating chamber
filter
temperature
cigarette
port
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黄海涛
王晋
李晶
孔维松
李雪梅
许�永
杨光宇
刘欣
杨叶昆
张承明
陈建华
耿永勤
张涛
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China Tobacco Yunnan Industrial Co Ltd
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China Tobacco Yunnan Industrial Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

The present invention relates to a kind of detection methods of royal jelly ingredient the amount of migration in filter stick, include the following steps:Step(1), puff number determine;Step(2), according to puff number set needed for heating chamber temperature;Step(3), suction;Step(4), constituent analysis.The present invention is eluted using purified air stream, eliminate the complicated smoke components background interference generated during practical cigarette burning, the precision and accuracy of measurement result significantly improve, and avoid the complex sample purification during conventional special flavoring filter stick ingredient is detected to flue gas migration analysis and enrichment procedure.The configuration of the present invention is simple, the situation of oral cavity suction temperatures cannot really be reflected by avoiding conventional temperature unanimously, reduce the influence of complicated flue gas.

Description

一种滤棒中蜂王浆成分迁移量的检测方法A detection method for the migration of royal jelly components in filter sticks

技术领域technical field

本发明涉及一种蜂王浆成分迁移量的检测方法,尤其是一种滤棒中蜂王浆成分迁移量的检测方法,属于烟用辅料的理化检验领域。The invention relates to a method for detecting the migration of royal jelly components, in particular to a method for detecting the migration of royal jelly components in filter sticks, and belongs to the field of physical and chemical testing of tobacco auxiliary materials.

背景技术Background technique

目前常用的特殊加香滤棒有多元复合加香滤嘴,爆珠滤嘴,香片滤嘴,加香料线滤嘴,颗粒加香滤嘴,成型纸加香滤嘴,三醋酸甘油酯加香滤嘴等。蜂王浆是工蜂采食花粉、花蜜后,由咽下腺和上颗腺分泌的,专供蜜蜂小幼虫和蜂王食用的浆状物。蜂王浆含有蛋白质、氨基酸、维生素、乙酞胆碱和有机酸等多种营养物质,是一种非常适宜人类的天然保健食品,具有多种医疗保健功能。目前咖蜂王浆在多元复合加香滤嘴,爆珠滤嘴,香片滤嘴,颗粒加香滤嘴等特殊加香滤嘴中有着广泛的应用。At present, the commonly used special flavoring filter sticks include multi-component compound flavoring filter, pop-bead filter, flavoring sheet filter, flavoring thread filter, particle flavoring filter, molded paper flavoring filter, triacetin flavoring filter etc. Royal jelly is a pulpy substance secreted by the hypopharyngeal and upper glands of worker bees after eating pollen and nectar, and is exclusively eaten by bee larvae and queen bees. Royal jelly contains proteins, amino acids, vitamins, acetylcholine and organic acids and other nutrients. It is a natural health food suitable for human beings and has various medical and health functions. At present, coffee royal jelly is widely used in special flavoring filters such as multi-component compound flavoring filters, pop-bead filters, flavoring slice filters, and granular flavoring filters.

目前特殊加香滤棒添加成分向卷烟烟气中迁移的测试方法通常采用吸烟机抽吸卷烟,再捕集烟气成分进行分析。由于卷烟燃烧时产生非常复杂的背景,会对特殊加香滤棒迁移成分的测定造成严重干扰,其成分的测定非常困难,分析结果的误差也非常大。如何真实准确的对特殊加香滤棒安全性成分进行准确的分析和检测成为烟草分析研究的重点。At present, the test method for the migration of ingredients added to special flavoring filter sticks into cigarette smoke usually uses a smoking machine to suck cigarettes, and then capture the smoke components for analysis. Due to the very complex background generated when the cigarette is burned, it will seriously interfere with the determination of the migration components of the special flavoring filter rod, the determination of its components is very difficult, and the error of the analysis results is also very large. How to truly and accurately analyze and detect the safety components of special flavoring filter sticks has become the focus of tobacco analysis research.

发明内容Contents of the invention

为了解决上述问题,本发明的目的在于提供一种滤棒中蜂王浆成分迁移量的检测方法。本发明的具体方案如下:In order to solve the above problems, the object of the present invention is to provide a method for detecting the migration of royal jelly components in filter sticks. Concrete scheme of the present invention is as follows:

一种滤棒中蜂王浆成分迁移量的检测方法,包括如下步骤:A method for detecting the migration of royal jelly components in a filter stick, comprising the steps of:

步骤(1)、抽吸口数确定Step (1), determine the number of suction ports

在待测卷烟的含有加香滤嘴的远唇端加料起始部位插入测温探针,在常规吸烟机上抽吸,通过测温探针测定每口抽吸时通过加香滤嘴起始部位烟气的温度,并确定整支卷烟的抽吸口数;Insert a temperature measuring probe into the starting part of the far lip end of the cigarette to be tested that contains the flavoring filter, smoke on a conventional smoking machine, and measure the starting position of the flavoring filter through the temperature measuring probe when each puff is smoked the temperature of the smoke and determine the number of puffs for the whole cigarette;

步骤(2)、根据抽吸口数设定所需加热腔的温度Step (2), set the temperature of the required heating chamber according to the number of suction ports

按卷烟实际抽吸温度设定检测装置的若干加热腔中的空气温度,并设定抽吸口数;Set the air temperature in several heating chambers of the detection device according to the actual smoking temperature of the cigarette, and set the number of suction ports;

步骤(3)、抽吸Step (3), suction

将吸烟机、烟气捕集器和滤嘴夹持器依次连接,把特种滤嘴卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件抽吸,抽吸的空气来自不同温度的加热腔,根据抽吸口数依次切换,每口抽吸通过过滤嘴的气流温度均和卷烟吸烟机实际抽吸时的气流温度一致;采用甲醇-乙腈溶液对模拟烟气进行烟气洗脱捕集;Connect the smoking machine, the smoke trap and the filter holder in sequence, remove the filter tip of the special filter cigarette from the cigarette, install it on the filter holder, start the smoking machine and smoke according to the standard conditions, The air sucked comes from heating chambers of different temperatures, which are switched sequentially according to the number of suction ports. The airflow temperature of each suction through the filter tip is consistent with the actual airflow temperature of the cigarette smoking machine; the simulated smoke is tested with methanol-acetonitrile solution. Flue gas elution and capture;

步骤(4)、成分分析;Step (4), component analysis;

对捕集液进行超高效液相色谱分析,分析条件:Perform ultra-high performance liquid chromatography analysis on the captured liquid, analysis conditions:

Symmetry 300TM C18,4.6 mm×250 mm, 5μm;Symmetry 300TM C18, 4.6mm×250mm, 5μm;

流动相为丙酮:1%醋酸溶液;0-3min为40:60,v/v;5-10min为70:30,v/v,梯度洗脱;流速: 1.5 mL/min;柱温40℃,进样量:10μL。The mobile phase is acetone: 1% acetic acid solution; 0-3min is 40:60, v/v; 5-10min is 70:30, v/v, gradient elution; flow rate: 1.5 mL/min; column temperature 40°C, Injection volume: 10 μL.

进一步地,使用检测装置进行检测,所述检测装置包括若干加热腔,加热腔一端连接进气口,另一端连接出气管,出气管围绕转盘设置,转盘上包括第一进气管,第一进气管随转盘转动,第一进气管一端在某一时刻与其中一个出气管连通,第一进气管另一端与第二进气管一端连通,第二进气管固定,另一端与滤嘴夹持器连接,滤嘴夹持器连接烟气捕集器,烟气捕集器连接吸烟机。Further, a detection device is used for detection. The detection device includes several heating chambers. One end of the heating chamber is connected to the air inlet, and the other end is connected to the air outlet pipe. The air outlet pipe is arranged around the turntable. As the turntable rotates, one end of the first air intake pipe communicates with one of the air outlet pipes at a certain moment, the other end of the first air intake pipe communicates with one end of the second air intake pipe, the second air intake pipe is fixed, and the other end is connected to the filter holder. The filter holder is connected with the smoke trap, and the smoke trap is connected with the smoking machine.

进一步地,加热腔为10个,加热腔上均设有温度调节装置,加热温度范围为30-200℃。Further, there are 10 heating chambers, each of which is equipped with a temperature regulating device, and the heating temperature range is 30-200°C.

进一步地,步骤(4)中,采用200ml甲醇-乙腈溶液对模拟烟气进行烟气洗脱捕集,其中,甲醇-乙腈的体积比为1:1。Further, in step (4), 200ml of methanol-acetonitrile solution is used to elute and trap the simulated flue gas, wherein the volume ratio of methanol-acetonitrile is 1:1.

与现有技术相比,本发明具有以下有益效果:Compared with the prior art, the present invention has the following beneficial effects:

(1)、本发明采用净化空气流进行洗脱,消除了实际卷烟燃烧过程中产生的复杂烟气成分背景干扰,测定结果的精密度和准确性显著提高。(1) The present invention adopts the purified air flow for elution, which eliminates the background interference of complex smoke components generated during the actual cigarette burning process, and significantly improves the precision and accuracy of the measurement results.

(2)、采用简单的顶空或溶剂提取就可直接进行分析,使得蜂王浆成分的测定变得非常容易,避免了常规特殊加香滤棒成分向烟气迁移分析检测中的复杂样品净化和富集操作。(2) Simple headspace or solvent extraction can be used for direct analysis, which makes the determination of royal jelly components very easy, and avoids the complicated sample purification and enrichment in the analysis and detection of conventional special flavored filter rod components to flue gas migration analysis. set operation.

(3)、本发明结构简单,操作方便,本发明的检测装置设置若干加热腔,设置不同的温度,可以非常好的人体口腔的抽吸温度,避免常规的温度一致不能真实反映口腔抽吸温度的情形,减少复杂烟气的影响。(3) The present invention is simple in structure and easy to operate. The detection device of the present invention is provided with several heating chambers, and different temperatures are set, so that the suction temperature of the human oral cavity can be very good, avoiding that the conventional temperature cannot truly reflect the suction temperature of the oral cavity situation, reducing the impact of complex smoke.

(4)、本发明的分析方法具有简便、快速、准确、灵敏度高、检测限低、有效可行,容易操作,准确灵敏,且测试周期相比现有检测方法缩短10-15分钟,具有推广应用价值。(4), the analysis method of the present invention is simple, fast, accurate, high sensitivity, low detection limit, effective and feasible, easy to operate, accurate and sensitive, and the test period is shortened by 10-15 minutes compared with the existing detection method, which has the advantages of popularization and application value.

附图说明Description of drawings

图1为本发明的检测装置的结构示意图;Fig. 1 is the structural representation of detection device of the present invention;

图1中:I为转盘;II为滤嘴夹持器;III为烟气捕集器;IV为吸烟机;V为空气入口;In Figure 1: I is the turntable; II is the filter holder; III is the smoke trap; IV is the smoking machine; V is the air inlet;

1-第一连通口,1’-第一加热腔;2-第二连通口,2’-第二加热腔;3-第三连通口,3’-第三加热腔;4-第四连通口,4’-第四加热腔;5-第五连通口,5’-第五加热腔;6-第六连通口,6’-第六加热腔;7-第七连通口,7’-第七加热腔;8-第八连通口,8’-第八加热腔;9-第九连通口,9’-第九加热腔;10-第十连通口,10’-第十加热腔;11-第一进气管;12-第二进气管。1-the first communication port, 1'-the first heating chamber; 2-the second communication port, 2'-the second heating chamber; 3-the third communication port, 3'-the third heating chamber; 4-the fourth communication 4'-the fourth heating chamber; 5-the fifth communication port, 5'-the fifth heating chamber; 6-the sixth communication port, 6'-the sixth heating chamber; 7-the seventh communication port, 7'- Seventh heating chamber; 8-eighth communication port, 8'-eighth heating chamber; 9-ninth communication port, 9'-ninth heating chamber; 10-tenth communication port, 10'-tenth heating chamber; 11-the first air intake pipe; 12-the second air intake pipe.

具体实施方式Detailed ways

下面结合附图和实施例对本发明作进一步的详细说明,但不以任何方式对本发明加以限制,基于本发明教导所做的任何变换或改进,均落入本发明的保护范围。实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用材料或设备未注明生产厂商者,均为可以通过购买获得的常规产品。The present invention will be described in further detail below in conjunction with the accompanying drawings and examples, but the present invention is not limited in any way, and any changes or improvements based on the teachings of the present invention fall within the protection scope of the present invention. If no specific technique or condition is indicated in the examples, it shall be carried out according to the technique or condition described in the literature in this field or according to the product specification. The materials or equipment used are not indicated by the manufacturer, and they are all conventional products that can be obtained through purchase.

实施例1Example 1

本实施例的检测装置,包括第一加热腔1’、第二加热腔2’、第三加热腔3’、第四加热腔4’、第五加热腔5’、第六加热腔6’、第七加热腔7’、第八加热腔8’、第九加热腔9’、第十加热腔10’,每个加热腔一端均连接进气口,另一端连接出气管,出气管围绕转盘I设置,形成围绕转盘I设置的第一连通口1、第二连通口2、第三连通口3、第四连通口4、第五连通口5、第六连通口6、第七连通口7、第八连通口8、第九连通口9、第十连通口10,转盘I上包括第一进气管11,第一进气管11随转盘I转动,第一进气管11一端在某一时刻与其中一个连通口连通,第一进气管11另一端与第二进气管12一端连通,第二进气管12固定,第二进气管12另一端与滤嘴夹持器II连接,滤嘴夹持器II连接烟气捕集器III,烟气捕集器III连接吸烟机IV,进气口一端可以设置进气管,进气管一端连接空气入口V。The detection device of this embodiment includes a first heating chamber 1', a second heating chamber 2', a third heating chamber 3', a fourth heating chamber 4', a fifth heating chamber 5', a sixth heating chamber 6', The seventh heating chamber 7', the eighth heating chamber 8', the ninth heating chamber 9', and the tenth heating chamber 10', one end of each heating chamber is connected to the air inlet, and the other end is connected to the air outlet pipe, and the air outlet pipe surrounds the turntable 1 Set to form the first communication port 1, the second communication port 2, the third communication port 3, the fourth communication port 4, the fifth communication port 5, the sixth communication port 6, the seventh communication port 7, The eighth communication port 8, the ninth communication port 9, the tenth communication port 10, the first air intake pipe 11 is included on the turntable 1, and the first air intake pipe 11 rotates with the turntable 1, and one end of the first air intake pipe 11 connects with it at a certain moment. One communication port communicates, the other end of the first air intake pipe 11 communicates with one end of the second air intake pipe 12, the second air intake pipe 12 is fixed, the other end of the second air intake pipe 12 is connected with the filter holder II, and the filter holder II Connect the smoke trap III, the smoke trap III is connected to the smoking machine IV, an air intake pipe can be arranged at one end of the air inlet, and one end of the air intake pipe is connected with the air inlet V.

加热腔上均设有温度调节装置,加热温度范围为30-200℃。加热腔上设有电子加热组件,可以迅速加热腔内空气至指定温度,精确控温。The heating chamber is equipped with a temperature regulating device, and the heating temperature range is 30-200°C. There is an electronic heating component on the heating chamber, which can quickly heat the air in the chamber to the specified temperature and control the temperature precisely.

转盘、抽烟机与控制系统连接,控制系统控制转盘自动旋转切换,且与抽烟机卷烟抽吸过程保持一致,即抽吸第一口时,第一连通口与第一进气管11相通;抽吸第二口时,切换至第二连通口,使得第二连通口与第一进气管11相通;依此类推,至抽吸第N口时,第N连通口与第一进气管11相通,转盘切换时,外界空气不会直接进入第一进气管,整个抽吸过程的空气均来自各个加热腔,高度真实模拟人体吸烟。The turntable and the smoking machine are connected with the control system, and the control system controls the automatic rotation and switching of the turntable, and is consistent with the cigarette smoking process of the smoking machine, that is, when the first puff is taken, the first communication port communicates with the first intake pipe 11; When the second port is used, switch to the second communication port so that the second communication port communicates with the first air intake pipe 11; When switching, the outside air will not directly enter the first air intake pipe, and the air in the entire suction process comes from each heating chamber, which highly simulates human smoking.

滤棒夹持器为圆周可调型滤嘴夹持器,其圆周可调,满足市售卷烟所有圆周规格。烟气捕集器为剑桥滤片捕集。所有组件间的气路为金属或玻璃隔热管路。The filter rod holder is a filter tip holder with adjustable circumference, and its circumference can be adjusted to meet all the circumference specifications of commercially available cigarettes. The smoke trap is a Cambridge filter. The gas paths between all components are metal or glass heat-insulated pipelines.

本实施例的用于特殊加香滤棒的蜂王浆成分迁移量的检测方法,使用上述检测装置按以下进行:The detection method of the royal jelly component migration amount used for the special flavoring filter stick of the present embodiment is carried out as follows using the above-mentioned detection device:

在A牌号加香复合滤嘴的卷烟装有加香滤嘴的远唇端加料起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过加香滤嘴起始部位的烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe at the far lip end of the cigarette with a flavored composite filter of A brand, and insert a temperature-measuring probe into it, smoke it on an ordinary smoking machine, and use the temperature-measuring probe to measure the amount of time passed during each puff. The temperature of the smoke at the beginning of the incense filter, and determine the number of puffs in the whole cigarette.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃) , heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber Chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把牌号A加香复合滤嘴的卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件(ISO抽吸模式)进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把加香复合滤嘴成分洗脱。Remove the filter tip of the brand A flavored compound filter cigarette from the cigarette, install it on the filter holder, start the smoking machine to smoke according to the standard conditions (ISO smoking mode), and when you take the first puff, The hot air in the first heating chamber passes through the filter stick; then it is switched by the turntable, when the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and elutes the components of the flavoring compound filter.

采用200ml甲醇-乙腈(1:1)溶液对模拟烟气进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。Use 200ml of methanol-acetonitrile (1:1) solution to carry out flue gas elution and trapping on the simulated flue gas. The collected solution was subjected to ultra-high performance liquid chromatography analysis.

分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速:1.5 mL/min;柱温40℃,进样量:10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5 mL/min; column temperature 40°C, injection volume: 10 μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

实施例2Example 2

本实施例的检测装置与实施例1相同,使用上述检测装置检测特殊加香滤棒的蜂王浆成分迁移量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the migration amount of the royal jelly component of the special perfuming filter stick is detected by using the above-mentioned detection device, as follows:

在B牌号含香料线滤嘴卷烟装有香料线的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过香料线部位烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe at the beginning of the fragrance-thread-containing filter cigarette of brand B, smoke it on an ordinary smoking machine, and use the temperature-measuring probe to measure the temperature of the smoke passing through the fragrance thread during each puff. And determine the puff number of the whole cigarette.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口35.4℃)、加热腔2’(第二口36.5 ℃)、加热腔3’(第三口40.1 ℃)、加热腔4’(第四口41.5 ℃)、加热腔5’(第五口43.6 ℃)、加热腔6’(第六口45.2 ℃)、加热腔7’(第七口47.1 ℃)。设定抽吸口数共7口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (the first port is 35.4°C), heating chamber 2' (the second port is 36.5°C) , heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), heating Chamber 7' (7th port 47.1°C). Set the number of suction ports to 7 in total.

把牌号B含香料线滤嘴卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把香料线成分洗脱。Remove the filter tip of brand B flavored line filter cigarette from the cigarette, install it on the filter holder, start the smoking machine and smoke according to the standard conditions. When taking the first puff, the one that passes through the filter stick is the first. The hot air in the heating chamber; then it is switched by the turntable, and the hot air in the second heating chamber passes through the filter rod when sucking the second port, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the fragrance line components.

采用200ml甲醇-乙腈(1:1)溶液对模拟烟气进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。Use 200ml of methanol-acetonitrile (1:1) solution to carry out flue gas elution and trapping on the simulated flue gas. The collected solution was subjected to ultra-high performance liquid chromatography analysis.

分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速:1.5mL/min;柱温40℃,进样量: 10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5mL/min; column temperature 40°C, injection volume: 10μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

实施例3Example 3

本实施例的检测装置与实施例1相同,使用上述检测装置检测特殊加香滤棒的蜂王浆成分迁移量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the migration amount of the royal jelly component of the special perfuming filter stick is detected by using the above-mentioned detection device, as follows:

在C牌号成型纸加香滤嘴的卷烟装有成型纸的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过成型纸起始部位的烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe into the initial part of the cigarette with the preformed paper and flavored filter of brand C, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the temperature that passes through the initial part of the preformed paper during each puff. The temperature of the smoke, and determine the number of puffs in the whole cigarette.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃) , heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber Chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把牌号C成型纸加香滤嘴的卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把加香成型纸成分洗脱。Remove the filter tip of the brand C shaped paper flavored filter cigarette from the cigarette, install it on the filter holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber; then switch through the turntable, and the hot air in the second heating chamber passes through the filter rod when sucking the second port, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the components of the flavored molding paper are eluted.

采用200ml甲醇-乙腈(1:1)溶液对模拟烟气进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。Use 200ml of methanol-acetonitrile (1:1) solution to carry out flue gas elution and trapping on the simulated flue gas. The collected solution was subjected to ultra-high performance liquid chromatography analysis.

分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速:1.5 mL/min;柱温40℃,进样量:10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5 mL/min; column temperature 40°C, injection volume: 10 μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

实施例4Example 4

本实施例的检测装置与实施例1相同,使用上述检测装置检测特殊加香滤棒的蜂王浆成分迁移量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the migration amount of the royal jelly component of the special perfuming filter stick is detected by using the above-mentioned detection device, as follows:

在D牌号含颗粒材料滤嘴卷烟装有颗粒材料的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过颗粒材料起始部位烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe into the starting part of D-brand filter cigarettes containing granular materials, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the amount of smoke that passes through the starting part of the granular material during each puff. temperature, and determine the number of puffs taken throughout the cigarette.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口35.4℃)、加热腔2’(第二口36.5 ℃)、加热腔3’(第三口40.1 ℃)、加热腔4’(第四口41.5 ℃)、加热腔5’(第五口43.6 ℃)、加热腔6’(第六口45.2 ℃)、加热腔7’(第七口47.1 ℃)。设定抽吸口数共7口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (the first port is 35.4°C), heating chamber 2' (the second port is 36.5°C) , heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), heating Chamber 7' (7th port 47.1°C). Set the number of suction ports to 7 in total.

把牌号D含颗粒材料滤嘴卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把颗粒材料成分洗脱。Remove the filter tip of the grade D filter cigarette containing particulate material from the cigarette, install it on the filter holder, start the smoking machine and smoke according to the standard conditions. When taking the first puff, the filter stick is the first The hot air in the heating chamber; then it is switched by the turntable, and the hot air in the second heating chamber passes through the filter rod when sucking the second port, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the particulate material components are eluted.

采用200ml甲醇-乙腈(1:1)溶液对模拟烟气进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。Use 200ml of methanol-acetonitrile (1:1) solution to carry out flue gas elution and trapping on the simulated flue gas. The collected solution was subjected to ultra-high performance liquid chromatography analysis.

分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速:1.5 mL/min;柱温40℃,进样量:10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5 mL/min; column temperature 40°C, injection volume: 10 μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

实施例5Example 5

本实施例的检测装置与实施例1相同,使用上述检测装置检测特殊加香滤棒的蜂王浆成分迁移量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the migration amount of the royal jelly component of the special perfuming filter stick is detected by using the above-mentioned detection device, as follows:

在E牌号三醋酸甘油酯加香滤嘴的卷烟装有滤嘴的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过滤嘴起始部位的烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe into the beginning of the filter on a cigarette with an E-brand triacetin flavored filter, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the beginning of each puff through the filter The temperature of the smoke, and determine the number of puffs of the whole cigarette.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃) , heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber Chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把牌号E三醋酸甘油酯加香滤嘴的卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把加香三醋酸甘油酯成分洗脱。Remove the filter tip of the brand E triacetin flavored filter cigarette from the cigarette, install it on the filter tip holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber is the hot air in the first heating chamber; then it is switched through the turntable, and when the second port is sucked, the hot air in the second heating chamber passes through the filter stick, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the flavored triacetin component.

模拟烟气采用200ml甲醇-乙腈(1:1)溶液进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速: 1.5 mL/min;柱温40℃,进样量: 10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。The simulated flue gas was eluted and captured with 200ml methanol-acetonitrile (1:1) solution. The collected solution was subjected to ultra-high performance liquid chromatography analysis. Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5 mL/min; column temperature 40°C, injection volume: 10 μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

实施例6Example 6

本实施例的检测装置与实施例1相同,使用上述检测装置检测特殊加香滤棒的蜂王浆成分迁移量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the migration amount of the royal jelly component of the special perfuming filter stick is detected by using the above-mentioned detection device, as follows:

在F牌号爆珠卷烟装有爆珠的部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过爆珠部位烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe into the part of the F-brand puffed-pear cigarette where the puffed-puff is installed, smoke it on an ordinary smoking machine, use the temperature-measured probe to measure the temperature of the smoke passing through the puff-puff part during each puff, and determine the temperature of the whole cigarette number of suction ports.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口35.4℃)、加热腔2’(第二口36.5 ℃)、加热腔3’(第三口40.1 ℃)、加热腔4’(第四口41.5 ℃)、加热腔5’(第五口43.6 ℃)、加热腔6’(第六口45.2 ℃)、加热腔7’(第七口47.1 ℃)。设定抽吸口数共7口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (the first port is 35.4°C), heating chamber 2' (the second port is 36.5°C) , heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), heating Chamber 7' (7th port 47.1°C). Set the number of suction ports to 7 in total.

把牌号F爆珠卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,捏破爆珠,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把爆珠中添加成分洗脱。Remove the filter tip of the brand F explosive bead cigarette from the cigarette, install it on the filter holder, pinch the explosive bead, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber; then switch through the turntable, when the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the added ingredients in the popping beads.

模拟烟气采用200ml甲醇-乙腈(1:1)溶液进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。The simulated flue gas was eluted and captured with 200ml methanol-acetonitrile (1:1) solution. The collected solution was subjected to ultra-high performance liquid chromatography analysis.

分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速: 1.5 mL/min;柱温40℃,进样量:10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5 mL/min; column temperature 40°C, injection volume: 10 μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

实施例7Example 7

本实施例的检测装置与实施例1相同,使用上述检测装置检测特殊加香滤棒的蜂王浆成分迁移量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the migration amount of the royal jelly component of the special perfuming filter stick is detected by using the above-mentioned detection device, as follows:

在G牌号含香片滤嘴的卷烟装有香片的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过香片部位烟气的温度,并确定整支卷烟的抽吸口数。Insert a temperature-measuring probe at the beginning of the cigarette with the flavor-filter on G brand cigarettes containing the flavor-filter filter, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the temperature of the smoke passing through the flavor-piece during each puff, and determine The number of puffs in a whole cigarette.

根据测得的抽吸温度及抽吸口数,设定检测装置中空气加热腔中的空气温度,其中,加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃) , heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber Chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把牌号G含香片滤嘴的卷烟的过滤嘴从卷烟上取下,安装到滤嘴夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为抽吸第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时通过滤棒的为抽吸第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,把香片成分洗脱。Remove the filter tip of the brand G cigarette containing flavor filter from the cigarette, install it on the filter holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber; then switch through the turntable, and the hot air in the second heating chamber is drawn through the filter rod when sucking the second port, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the ingredients of the flavor sheet.

模拟烟气采用200ml甲醇-乙腈(1:1)溶液进行烟气洗脱捕集。将捕集液,进行超高效液相色谱分析。分析条件:Symmetry 300TM C18(4.6 mm×250 mm, 5μm);流动相为丙酮:1%醋酸溶液,0-3min(40:60,v/v),5-10min(70:30,v/v),梯度洗脱,流速: 1.5 mL/min;柱温40℃,进样量:10μL。其余与实施例1相同,蜂王浆成分分析结果见表1。The simulated flue gas was eluted and captured with 200ml methanol-acetonitrile (1:1) solution. The collected solution was subjected to ultra-high performance liquid chromatography analysis. Analysis conditions: Symmetry 300TM C18 (4.6 mm×250 mm, 5 μm); mobile phase is acetone: 1% acetic acid solution, 0-3min (40:60, v/v), 5-10min (70:30, v/v ), gradient elution, flow rate: 1.5 mL/min; column temperature 40°C, injection volume: 10 μL. The rest are the same as in Example 1, and the analysis results of the components of royal jelly are shown in Table 1.

表1蜂王浆成分分析结果Table 1 Analysis results of royal jelly components

由表1可以看出,样品不受复杂的烟气影响,可真实反映滤嘴中蜂王浆成分的含量。It can be seen from Table 1 that the sample is not affected by complex smoke and can truly reflect the content of royal jelly in the filter.

可见,使用本实施例的检测装置和方法能对特殊加香滤嘴中蜂王浆成分迁移量进行准确分析,使样品的分析灵敏度提高,检测周期更短,并能有效指导产品开发及设计。It can be seen that using the detection device and method of this embodiment can accurately analyze the migration of royal jelly components in special flavoring filters, improve the analysis sensitivity of samples, shorten the detection cycle, and effectively guide product development and design.

以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,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 above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of the present invention. within the scope of protection.

Claims (4)

1. the detection method of royal jelly ingredient the amount of migration in a kind of filter stick, it is characterised in that:Include the following steps:
Step(1), puff number determine
It is inserted into thermoprobe at the remote lip end charging starting position containing Flavoring filter of cigarette to be measured, is taken out on conventional smoking machine It inhales, originates the temperature of position flue gas when measuring every mouthful of suction by thermoprobe by Flavoring filter, and determine whole branch cigarette Puff number;
Step(2), according to puff number set needed for heating chamber temperature
The air themperature in several heating chambers of detection device is set by the practical suction temperatures of cigarette, and sets puff number;
Step(3), suction
Smoking machine, Fume collector and filter tip clamper are sequentially connected, the filter tip of extraordinary filter tip cigarette is taken from cigarette Under, it is installed on filter tip clamper, starts smoking machine and aspirated by standard conditions, heating of the air from different temperatures of suction Chamber switches successively according to puff number, and every mouthful of gas flow temperature for being aspirated through filter tip is and when the practical suction of cigarette smoking machine Gas flow temperature it is consistent;Flue gas elution trapping is carried out to simulated flue gas using methanol-acetonitrile solution;
Step(4), constituent analysis;
After trapping, ultra performance liquid chromatography analysis, analysis condition are carried out to trapping solution:
Symmetry 300TM C18,4.6 mm × 250 mm, 5 μm;
Mobile phase is acetone:1% acetum;0-3min is 40:60, v/v;5-10min is 70:30, v/v, gradient elution;Stream Speed: 1.5 mL/min;40 DEG C of column temperature, sample size:10μL.
2. detection method according to claim 1, it is characterised in that:It is detected using detection device, the detection dress It sets including several heating chambers, heating chamber one end connects air inlet, and the other end connects escape pipe, and escape pipe is arranged around turntable, turns Include the first air inlet pipe on disk, the first air inlet pipe is rotated with turntable, and first air inlet pipe one end at a time goes out with one of them Tracheae is connected to, and the first air inlet pipe other end is connected to second air inlet pipe one end, and the second air inlet pipe is fixed, and the other end is clamped with filter tip Device connects, and filter tip clamper connects Fume collector, and Fume collector connects smoking machine.
3. detection method according to claim 1, it is characterised in that:Heating chamber is 10, and temperature is equipped in heating chamber Regulating device, heating temperature range are 30-200 DEG C.
4. detection method according to claim 1, it is characterised in that:Step(4)In, using 200ml methanol-acetonitrile solution Flue gas elution trapping is carried out to simulated flue gas, wherein the volume ratio of methanol-acetonitrile is 1:1.
CN201810467705.2A 2018-05-16 2018-05-16 The detection method of royal jelly ingredient the amount of migration in a kind of filter stick Pending CN108627583A (en)

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