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当前位置:首页>>新闻中心>>公司新闻>>进出口食品中环己基氨基磺酸钠抽取检验过程
进出口食品中环己基氨基磺酸钠抽取检验过程
来源:http://www.jnjrh.com 日期:2019-05-29 发布人:admin
1 范围
1 Scope
本规范规则了食品中环己基氨基磺酸钠(甘美素)检验的制样和液相色谱-质谱-质谱法。
This specification regulates the preparation of samples for the determination of sodium cyclohexylaminosulfonate (glycerin) in food and the method of liquid chromatography-mass spectrometry-mass spectrometry.
本规范适用于水果罐头、浓缩山葡萄汁、白酒、糕点、糖果、甜面酱、酱菜中环己基氨基磺酸钠的检测和确证。
This specification is applicable to the detection and confirmation of sodium cyclohexylaminosulfonate in canned fruits, concentrated mountain grape juice, liquor, cakes, candy, sweet paste and pickles.
2 办法提要
Summary of two approaches
试样用水超声提取,离心后,上清液供液相色谱-质谱/质谱仪检测,外标法定量。
After centrifugation, the supernatant was detected by liquid chromatography-mass spectrometry/mass spectrometry and quantified by external standard method.
3 试剂和资料
3 reagents and information
除另有规则外,一切试剂均为剖析纯,水为超纯水:
Except for other rules, all reagents are analytical pure and water is ultrapure water.
3.1 乙酸。
3.1 acetic acid.
3.2 乙腈:液相色谱纯。
3.2 Acetonitrile: Pure by liquid chromatography.
3.30.1%乙酸水溶液(体积分数):量取乙酸4 mL。用水稀释至4000 mL。
3.30.1% acetic acid aqueous solution (volume fraction): acetic acid 4 mL. Dilute to 4000 mL with water.
3.4环己基氨基磺酸钠规范品(Sodium Cyclamate, C6H12NNaO3S,CAS号:139-05-9):纯度大于等于99%。
3.4 Sodium Cyclamate (C6H12NNaO3S, CAS No. 139-05-9): Purity greater than or equal to 99%.
3.5 环己基氨基磺酸钠规范储藏液:精确称取适量环己基氨基磺酸钠规范品,用水配制成浓度为500 ug/mL,的规范储藏溶液。该溶液在。0℃~4℃冰箱中保管。
3.5 Sodium Cyclohexyl Aminosulfonate Specification Storage Fluid: Accurately weigh the appropriate amount of Sodium Cyclohexyl Aminosulfonate Specification, and prepare the standard storage solution with water concentration of 500 ug/mL. The solution is in. Keep in refrigerator at 0 ~4 C.
3.6 环己基氨基磺酸钠规范中间液:精确移取一定体积的环己基氨基磺酸钠规范储藏液,用水配制成浓度为1ug/mL的规范中间液,该溶液在0℃~4℃冰箱中保管。
3.6 Sodium Cyclohexyl Aminosulfonate Specification Intermediate: Accurate removal of a certain volume of Sodium Cyclohexyl Aminosulfonate Specification Storage Fluid, prepared with water concentration of 1 ug/mL, the solution is stored in the refrigerator at 0 ~4 ~C.
3.7 环己基氨基磺酸钠规范工作溶液:精确移取一定体积的规范中间液,可依据需求用水稀释成适用浓度的规范工作液。该溶液在0℃~4℃冰箱中保管。
3.7 Sodium Cyclohexyl Aminosulfonate Standard Working Solution: Accurate removal of a certain volume of normative intermediate liquid, according to the demand of water dilution into the applicable concentration of normative working fluid. The solution is kept in a refrigerator at 0 ~4 C.
3.80.45 um滤膜(水相)。
3.80.45 um membrane (aqueous phase).
氨基磺酸
4 仪器和设备
4 Instruments and equipment
4.1液相色谱串联质谱仪:配有电喷雾(ESI)离子源。
4.1 liquid chromatography tandem mass spectrometry: equipped with an electrospray ionization (ESI) ion source.
4.2 混匀器。
4.2 mixer.
4.3 超声波提取器。
4.3 Ultrasound extractor.
4.4 离心机。
4.4 Centrifuge.
5 试样制备与保管
Sample preparation and storage
5.1 试样制备
5.1 Sample Preparation
5.1.1 水果罐头类
5.1.1 Canned fruits
将所取原始样品在室温下开罐,将罐内液体和固体物分开并分别称量。依照两者比例取1kg代表性样品,经组织捣碎机捣碎,再将混匀样品分安装干净容器内密封,作为试样,并标明标志。
The original sample was opened at room temperature, and the liquid and solid in the tank were separated and weighed separately. According to the ratio of the two, 1 kg representative sample is taken, and the sample is smashed by tissue rammer. Then the homogenized sample is separately sealed in a clean container, which is used as the sample and marked.
5.1.2 酒类、果汁类
5.1.2 Wines and Juices
将所取原始样品1 kg在瓷混样桶内充沛混匀,再将混匀样品分安装干净容器内密封,作为试样,标明标志。
The original sample 1 kg was fully mixed in the pottery mixing barrel, and then the homogenized sample was separately installed in a clean container and sealed as a sample, marking.
5.1.3 糕点类、糖果类
5.1.3 Pastry and confectionery
取有代表性样品1 kg。将样品按四分法缩至200g,在玻璃研钵中研碎。再将混匀样品分安装干净容器内密封,作为试样,并标明标志。
The representative sample was 1 kg. Shrink the sample to 200 g by quartering and grind it in a glass bowl. The mixing sample is then separated into clean containers, sealed and marked as the sample.
5.1.4 甜面酱类、酱菜类
5.1.4 Sweet noodle sauces and pickles
取有代表性样品1 kg,将样品按四分法缩至500g,所取样品经组织捣碎机捣碎。再将混匀样品分安装干净容器内密封,作为试样,并标明标志。
The representative sample was taken for 1 kg. The sample was reduced to 500 g by quartile method. The sample was crushed by tissue rammer. The mixing sample is then separated into clean containers, sealed and marked as the sample.
5.2 试样保管
5.2 Sample Storage
样于0℃~4℃保管。在抽样及制样的操作过程中,应避免样品遭到污染或发作含量的变化。
Samples are stored at 0 ~4 C. In the process of sampling and sample preparation, it is necessary to avoid contamination of the sample or changes in the content of the sample.
6 测定步骤
6 determination steps
6.1 提取
6.1 extraction
6.1.1 水果罐头、糕点、糖果、甜面酱、酱菜、果汁类样品
6.1.1 Samples of canned fruits, cakes, candies, sweet paste, pickles and juices
称取试样约1g(准确至0.01g)置于25 mL、离心管中,参加8.0 mL水,混匀后,于超声波清洗器中超声20 min后,于4000 r/min离心5 min。过滤并用水定容至10mL,容量瓶中,取局部过0.45um滤膜,供液相色谱-质谱质谱仪测定。
The sample is weighed about 1g (accurate to 0.01g) and placed in a 25 mL centrifugal tube. The sample is mixed with 8.0 mL water. After 20 minutes of ultrasound in an ultrasonic cleaner, the sample is centrifuged for 5 minutes at 4000 r/min. Filtration was carried out with water at a constant volume of 10 mL. In the volumetric bottle, a local over 0.45 um filter membrane was taken for determination by liquid chromatography-mass spectrometry.