Gas chromatography-positive chemical ionization-tandem triple quadruple mass spectrometry (GC-PCI-MS/MS) was established for the determination of ethyl carbonate in breads. After spiked with internal standard of ethyl carbamate, samples were extracted and precipitated by 10% lead acetate solution, purified by Cleanert EC alkaline diatomite solid phase extraction column. The extracted solution was detected by GC-PCI-MS/MS in multiple reaction monitoring (MRM) mode. And the internal standard method was used for quantification. The results showed that the developed method exhibited good linear over the range from 0.5 μg/L to 50.0 μg/L with a correlation coefficient of 0.999 5. The limit of detection (LOD) was 0.12 μg/kg and the limit of quantification (LOQ) was 0.40 μg/kg. The recoveries at three spiked levels of 2.0, 10.0 and 50.0 μg/kg were between 89.3% and 95.6% with the intra-day relative standard deviations (RSD) (n=6) from 1.3% to 4.6% and the inter-day relative standard deviations (RSD) (n=6) from 4.5% to 9.9%. The proposed method is rapid, accurate, has strong selectivity and characterized with acceptable sensitivity and accuracy to meet the requirements of ethyl carbonate analysis in breads.
HUANG Minxing
,
GAO Yufeng
,
ZHEN Zhenpeng
,
LI Shuocong
,
PANG Yanghai
,
WANG Xiaopeng
,
YU Goubin
. Determination of ethyl carbamate in breads by GC-PCI-MS/MS[J]. Food and Fermentation Industries, 2020
, 46(1)
: 269
-273
.
DOI: 10.13995/j.cnki.11-1802/ts.021877
[1] 龙顺荣,周勇,郦明浩,等.发酵食品中氨基甲酸乙酯污染状况调查与分析[J]. 食品与发酵工业, 2013,39(2):196-199.
[2] 周凯,唐冰娥,徐振林,等.发酵食品中氨基甲酸乙酯形成机理和快速检测方法研究进展[J]. 生物加工过程, 2018, 16(2): 31-41.
[3] ZHANG J R, FANG F, CHEN J, et al. The arginine deiminase pathway of koji bacteria is involved in ethyl carbamate precursor production in soy sauce[J]. FEMS Microbiol Lett, 2014,358(1):91-97.
[4] 刘会昌,石建新.氨基甲酸乙酯诱导HepG2细胞凋亡的分子机制[J]. 食品科学, 2018,39(17):159-164.
[5] CUI X, WANG J J, QIU N N, et al.In vitro toxicological evaluation of ethyl carbamate in human Hep G2 cells[J].Toxicology Research, 2016, 5(2):697-702.
[6] CHUN S H, CHA Y N, KIM C.Urethane increases reactive oxygen species and activates extracellular signal-regulated kinase in RAW 264.7 macrophages and A549 lung epithelial cells[J].Archives of Pharmacal Research,2013,36(6):775-782.
[7] CHEN W, XU Y, ZHANG L X, et al. Blackberry subjected to in vitro gastrointestinal digestion affords protection against Ethyl Carbamate-induced cytotoxicity[J]. Food Chemistry, 2016, 212(1):620-627.
[8] 魏玉洁,付方圆,武顺,等.葡萄酒酵母car1基因表达量与EC含量相关性的研究[J].食品与发酵工业,2015,41(8):59-64.
[9] ZHOU W Y, FANG R S, CHEN Q H. Effect of gallic and protocatechuic acids on the metabolism of ethyl carbamate in Chinese yellow rice wine brewing [J]. Food Chemistry, 2017, 233(10): 174-181.
[10] WEBER J V, SHARYPOV V I. Ethyl carbamate in foods and beverages: a review[J]. Environmental Chemistry Letters, 2009, 7(3):233-247.
[11] BAAN R, STRAIF K, GROSSE Y, et al. Carcinogenicity of alcoholic beverages.[J]. Lancet Oncology, 2007, 8(4):292-293.
[12] 肖泳, 邓放明. 发酵食品中氨基甲酸乙酯的研究进展[J]. 食品安全质量检测学报, 2012(3):216-221.
[13] STEFANI E D, BOFFETTA P, DE H, et al. The effect of smoking and drinking in oral and pharyngeal cancers: A case-control study in Uruguay[J].Cancer Lett, 2007, 246(1): 282-289.
[14] 黄振波.气相色谱法测定酒中氨基甲酸乙酯[J].现代食品,2016,3(6):74-76.
[15] 蒙法双.气相色谱法测定饮料酒中氨基甲酸乙酯的含量[J].食品安全导刊,2016(9):77-77.
[16] 雒丽娜,王颖,张妮娜,等.固相萃取-气相色谱-质谱法测定酸奶中氨基甲酸乙酯[J].中国卫生检验杂志,2015,25(18):3 070-3 071.
[17] 张万利,梁新红,冉军舰,等. SLE结合GC-MS法测定葡萄酒中氨基甲酸乙酯[J]. 中国酿造, 2017, 36(1):176-179.
[18] 张雅琪,王蒙,孔红建,等.固相萃取-气相色谱-质谱法测定腐乳中氨基甲酸乙酯[J].食品安全质量检测学报,2018,9(3):609-613.
[19] GB 5009.223—2014,食品安全国家标准食品中氨基甲酸乙酯的测定[S].北京:中国标准出版社,2014.
[20] 柯润辉,王丽娟,安红梅,等.超高效液相色谱-串联质谱法同时测定白酒中氨基甲酸乙酯和8种甜味剂[J].食品与发酵工业,2016,42(4):174-178.
[21] 徐小民,何华丽,阮宇迪,等.气相色谱-三重四极杆串联质谱法同时测定调味品中的氨基甲酸乙酯和氯丙醇[J].色谱,2013,31(11):1 129-1 133.
[22] KIM E, LEE J, CHOI S, et al. Analysis of ketamine and norketamine in urine by automatic solid-phase extraction(SPE) and postive ion chemical ionization-gas chromatography-mass spectrometry(PCI-GC-MS)[J]. Forensic Science International, 2008,174(2):197-202.
[23] 司晓喜,张凤梅,朱瑞芝,等.气相色谱-正化学电离源-飞行时间质谱法测定烟草吸食者唾液中的吡嗪和吡啶类物质[J].质谱学报,2018,39(4):467-475.
[24] 幸苑娜,王欣,陈泽勇,等.气相色谱-正化学源质谱法测定家用橡胶手套中7种N-亚硝胺及其前体物的迁移量[J].分析测试学报,2011,30(5):503-508.
