Determination of 3-Acetyl-2,5-dimethylthiophene in Food Flavor by Gas Chromatography-Triple Quadrupole Mass Spectrometry
摘 要
称取约0.1 g样品,加入约6 mL正庚烷,超声提取15 min,静置冷却后用正庚烷定容至10.0 mL,混匀后静置数分钟,取上清液过0.22 μm有机相滤膜后,采用Agilent HP-INNOWax毛细管柱(30 m×0.25 mm,0.25 μm)进行分离,质谱中选择电子轰击离子源和多反应监测模式。3-乙酰基-2,5-二甲基噻吩的质量浓度在0.010~2.00 mg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.1 mg·kg-1。以稀膏状香精样品为基质进行加标回收试验,3-乙酰基-2,5-二甲基噻吩的回收率在82.7%~92.9%之间,测定值的相对标准偏差(n=6)在0.70%~2.8%之间。以不同类型的香精样品为基质进行加标回收试验,回收率在92.2%~107%之间。
Abstract
The sample (about 0.1 g) was ultrasonically extracted with about 6 mL of n-heptane for 15 min, and the mixture was let stand for cooling, and then made up to 10.0 mL with n-heptane. After the mixture was mixed well and let stand for several minutes, the supernatant was taken and filtrated with 0.22 μm organic filter membrane. An Agilent HP-INNOWax capillary column (30 m×0.25 mm, 0.25 μm) was used for separation, and electron bombardment ion source and multi-reaction monitoring mode were selected in mass spectrometry. The peak area of 3-acetyl-2,5-dimethylthiophene was kept linear with its mass concentration in the range of 0.010-2.00 mg·L-1, and the detection limit (3S/N) was 0.1 mg·kg-1. Tests for recovery obtained by standard addition mehtod was carried out with the thin paste flavor samples as the matrix, giviny results in the range of 82.7%-92.9%, and the relative standard deviation (n=6) of the measured values were between 0.70% and 2.8%. Values of recovery was between 92.2% and 107%, with different types of flavor samples as the matrix.
中图分类号 O657.6 DOI 10.11973/lhjy-hx201903016
所属栏目 工作简报
基金项目 浙江省食品药品监督管理局2016年度食品药品科技计划项目(SP201604)
收稿日期 2018/6/9
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备注茅佩卿,工程师,主要从事食品理化检测研究工作
引用该论文: MAO Peiqing,JIN Shaoqiang,WANG Zhanhua,ZHU Bingqi,XU Xiaoying,LUO Jinwen. Determination of 3-Acetyl-2,5-dimethylthiophene in Food Flavor by Gas Chromatography-Triple Quadrupole Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(3): 328~332
茅佩卿,金绍强,王展华,朱炳祺,徐潇颖,罗金文. 气相色谱-三重四极杆质谱法测定食用香精中3-乙酰基-2,5-二甲基噻吩[J]. 理化检验-化学分册, 2019, 55(3): 328~332
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参考文献
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【2】EFSA Panel on Additives and Products or Substances used in Animal Feed. Scientific opinion on the safety and efficacy of thiazoles, thiophene, thiazoline and thienyl derivatives (chemical group 29):3-Acetyl-2,5-dimethylthiophene when used as a flavouring for all animal species[J]. EFSA Journal, 2013,11(8):3323-3336.
【3】广西中烟工业有限责任公司.一种食用香精香料中3-乙酰基-2,5-二甲基噻吩的测定方法:CN104655775B[P]. 2017-01-04.
【4】广西中烟工业有限责任公司.一种食品添加剂中3-乙酰基-2,5-二甲基噻吩的测定方法:CN104655753A[P]. 2015-05-27.
【5】CANNON R J, HO C T. Volatile sulfur compounds in tropical fruits[J]. Journal of Food and Drug Analysis, 2018,26(2):445-448.
【6】HERNANDEZ F, PORTOLES T, PITARCH E, et al.Potential of gas chromatography coupled to triple quadrupole mass spectrometry for quantification and confirmation of organohalogen xenoestrogen compounds in human breast tissues[J]. Analytical Chemistry, 2005,77(23):7662-7672.
【7】HUO L G, LI H D, ZHAO C L, et al. The determination of PCBs in meat and sea food by GC-QqQ-MS/MS[J]. Food Analytical Methods, 2012,5(6):1481-1491.
【8】KALACHOVA K, PULKRABOVA J, CAJKA T, et al. Gas chromatography-triple quadrupole tandem mass spectrometry:A powerful tool for the (ultra)trace analysis of multiclass environmental contaminants in fish and fish feed[J]. Analytical and Bioanalytical Chemistry, 2013,405(24):7803-7815.
【9】LEANDRO C C, FUSSELL R J, KEELY B J. Determination of priority pesticides in baby foods by gas chromatography tandem quadrupole mass spectrometry[J]. Journal of Chromatography A, 2005,1085(2):207-212.
【10】PATEL K, FUSSELL R J, HETMANSKI M, et al. Evaluation of gas chromatography-tandem quadrupole mass spectrometry for the determination of organochlorine pesticides in fats and oils[J]. Journal of Chromatography A, 2005,1068(2):289-296.
【11】余卫军,王佩,邱月生,等.气相色谱-三重四极杆质谱联用法检测市售腊肠中9种挥发性亚硝胺[J].分析测试学报, 2016,35(6):719-723.
【12】胡光辉,刘伟丽,钱冲,等.气相色谱技术在食品安全检测中的应用[J].食品安全质量检测学报, 2016,7(11):4312-4317.
【13】邓晓君,胡国华,朱坚,等.气相色谱-离子阱二级质谱测定食品中丙烯酰胺残留[J].理化检验-化学分册, 2007,43(4):256-259.
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