GC-MS∕MS测定不同食品中氨基甲酸甲酯及氨基甲酸乙酯的含量.pdf

2018年2月
食品研究与开发
第39卷第3期
Food Research And Development
标准与检测
162ー
DOI:10.3969/jsn.1005-6521.2018.03.029
GC-MS/MS测定不同食品中氨基甲酸甲酯及
氮基甲酸乙酯的含量
周佳,成长玉,郭庆1,陈祥贵
(1.四川省食品药品检验检测院,四川成都611731;2.西华大学食品与生物工程学院,
四川成都610039)
摘要:建立内标法同时测定固体半固体及液体基质中氨基甲酸甲酯及氪基甲酸乙酯含量的气相一质语/质语(Gas
chromatography- ass/Mass,C-MSMS)方法。以D、ー氯基甲酸乙酯为内标,米用CC- MS/MS多反应监测模式( Multiple
Reaction Monitoring,MRM模式);毛细管色谱柱:DB- INNOWAX,30mx0.25mm(内径)x0.25um(膜厚);进样方式:脉
冲不分流;进样量:1L;柱温:80℃保持2min,以10℃min至180℃保持3min,240℃后运行6min;流速1.0mL/mina氮
基甲酸甲酯在20 ng/mi.~1l00 ng/ml,魚基甲酸乙在10ngnl~500 ng/ml.范国内线性关系良好。相关系数分别为
0.9987和0.9999液体基质平均回收率为78.4%及100.20%:固体及半固体基质平均回收率为62.48%及100.49%
检出限分別为6ugkg及3pgkg。本方法灵敏度高,专属性强,稳定性好,准确度高
关键词:氨基甲酸甲酯;氮基甲酸乙酯;C-MS/MS;固体半固体基质
Simultaneous Determination of Methyl Carbamate and Ethyl Carbamate in Different Food by GC-MS/MS
ZHOU Jia CHENG Chang-yu, GUO Qing, CHEN Xiang-gui
(1. Sichuan Institute for Food and Drug Conlrol, Chengdu 611731, Sichuan, China; 2. School of Food and
Biological Egineering, Xihua University, Chengdu 610039, Sichuan, China
Abstract: To establish a method for simultaneous determination of methyl carbamate and ethyl carbamate in
solid, semisolid and liquid substrates with internal standard by GC-MS/MS. Ethyl carbamale-ds was used as in
ternal standard Multiple reaction monitoring(MRM)mode was employed by GC-MS/MS Chromatographic
separation was performed on a Db-innowax capillary column(30 mx0.25 mmx.25 wm) Pulse splitless njec
tion mode was used and the injection volume is I WL. The temperature program was set as: the initial tempera
ture was 80 C, holding for 2 min, then 10 C/min up to 180 C, holding for3 min, 240 C post run 6 min. Flow
rale was 1.0 mi /min. The developed method showed good linearity in the range of 20 ng/m-1000 ng/m, for
methyl carbamate(=0.998 7), 10 n/ml-500 ng/ml for ethyl carbamate (r=0. 9999 ) respectively. The aver
age recoveries of methyl carbamate and ethyl carbamate in liquid substrates were 78.4 and 100.20%o, respec
tively. The average recoveries of methyl carbamate and ethyl carbamate in solid and semisolid substrates were
62. 48 and 100. 49 % .The limits of detection were 6 wgkg and 3 wg/kg respectively. The methods of simulta-
neous determination of methyl carbamate and ethyl carbamate in different substrates by GC-MS/MS is proved Lo
be sensitive, specific stable and accurate
Key words: methyl carbamate; ethyl carbamate; GC-MS/MS; solid and semisolid substrates
引文格式:
周佳,成长玉,郭庆,等.CC- MS/MS测定不同食品中氮基甲酸甲酯及基甲酸乙酯的含量J食品研究与开发,2018,39
(3):162-167
ZHOUJIA, CHENG Changyu, GLO Qing, ct al. Simultancous Determination of Methyl Carbamate and Ethyl Carbamate in
Different Food by GC-MS/MS[J]. Food Research and Development, 2018, 39(3): 162-167
基金项日:四川省省部学科开放课题项日(si2015-010)
作者简介:周(1983-),女(汉),主管药师,硕1,研究方向:食品檢验。
万方数据