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
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摘要
称取约0.1g样品,加入约6mL正庚烷,超声提取15min,静置冷却后用正庚烷定容至10.0mL,混匀后静置数分钟,取上清液过0.22μm有机相滤膜后,采用Agilent HP-INNOWax毛细管柱(30m×0.25mm,0.25μm)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0.1mg·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。
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 0.22μm organic filter membrane.An Agilent HP-INNOWax capillary column(30 m×0.25 mm,0.25μm) 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(3 S/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.
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 0.22μm organic filter membrane.An Agilent HP-INNOWax capillary column(30 m×0.25 mm,0.25μm) 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(3 S/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.
引文
[1] 张华.几个杂环类香料新产品在香精中的应用.第二届全国香料香精化妆品洗涤用品食品添加剂专题学术论坛会议[C].上海:[出版者不详],2011:70-72.
[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.
[14] GB/T 27404-2008 实验室质量控制规范食品理化检测[S].
[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.
[14] GB/T 27404-2008 实验室质量控制规范食品理化检测[S].