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张家宁,丁轲,韩涛,郭思梦,陈湘宁.液质联用法检测饼干中4种单端孢霉烯类真菌毒素[J].食品安全质量检测学报,2015,6(6):2179-2187

液质联用法检测饼干中4种单端孢霉烯类真菌毒素

Determination of 4 kinds of trichothecenes in cookies by high performance liquid chromatography- mass spectrometry/mass spectrometry

投稿时间：2015-05-13 修订日期：2015-06-01

DOI：

中文关键词: 单端孢霉烯类真菌毒素液相色谱-串联质谱法饼干

英文关键词:trichothecenes liquid chromatography-mass spectrometry/mass spectrometry cookies

基金项目:北京市自然科学基金项目(14L00184)、北京市属高校青年拔尖人才培育计划项目(CIT&TCD20154045)、食品质量与安全北京实验室2015年度开放课题、2015年北京农学院学位与研究生教育改革与发展项目(2015YJS034)

作者	单位
张家宁	北京农学院食品科学与工程学院; 食品质量与安全北京实验室; 农产品有害微生物及农药残留安全检测与控制北京市重点实验室
丁轲	北京农学院食品科学与工程学院; 食品质量与安全北京实验室; 农产品有害微生物及农药残留安全检测与控制北京市重点实验室
韩涛	北京农学院食品科学与工程学院; 食品质量与安全北京实验室; 农产品有害微生物及农药残留安全检测与控制北京市重点实验室
郭思梦	北京农学院食品科学与工程学院;食品质量与安全北京实验室; 农产品有害微生物及农药残留安全检测与控制北京市重点实验室
陈湘宁	北京农学院食品科学与工程学院; 食品质量与安全北京实验室; 农产品有害微生物及农药残留安全检测与控制北京市重点实验室

Author	Institution
ZHANG Jia-Ning	Department of Food Science and Engineering, Beijing University of Agriculture; Beijing Laboratory of Food Quality and Safety; Beijing Key Laboratory of Agricultural Product Detection and Control of Spoilage Organisms and Pesticide Residue
DING Ke	Department of Food Science and Engineering, Beijing University of Agriculture; Beijing Laboratory of Food Quality and Safety; Beijing Key Laboratory of Agricultural Product Detection and Control of Spoilage Organisms and Pesticide Residue
HAN Tao	Department of Food Science and Engineering, Beijing University of Agriculture; Beijing Laboratory of Food Quality and Safety; Beijing Key Laboratory of Agricultural Product Detection and Control of Spoilage Organisms and Pesticide Residue
GUO Si-Meng	Department of Food Science and Engineering, Beijing University of Agriculture; Beijing Laboratory of Food Quality and Safety; Beijing Key Laboratory of Agricultural Product Detection and Control of Spoilage Organisms and Pesticide Residue
CHEN Xiang-Ning	Department of Food Science and Engineering, Beijing University of Agriculture; Beijing Laboratory of Food Quality and Safety; Beijing Key Laboratory of Agricultural Product Detection and Control of Spoilage Organisms and Pesticide Residue

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中文摘要:

目的建立饼干中4种单端孢霉烯类真菌毒素的液相色谱-质谱联用分析方法。方法样品经乙腈/水溶液(84:16, V:V)提取后用MycoSep?227或 MycoSep?226多功能柱净化, Agilent ZORBAX Bonus-RP色谱柱分离, 液相色谱-质谱联用(LC-MS/MS)测定, 电喷雾正离子模式(ESI+)和负离子模式(ESI－)多反应模式检测。结果样品中4种单端孢霉烯类真菌毒素在各自的线性范围内线性关系良好, 相关系数均不低于0.997, 定量限为5~20 μg/kg, 3个加标水平下平均回收率为66.9%~101.8%, 相对标准偏差为3.7%~13.9%。结论该方法具有前处理简单、净化效果好、灵敏度高, 适用于同时检测一种样品中4种单端孢霉烯类真菌毒素的残留量。

英文摘要:

Objective To establish a simultaneous determination method for 4 kinds of trichothecenes in cookies by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were sequentially extracted by 84% acetonitrile-water solution(V:V), cleaned up with MycoSep?227 or MycoSep?226, and separated by Agilent ZORBAX Bonus-RP column and detected by LC-MS/MS. The MS conditions used were negative (ESI+) and positive (ESI－) electrospray ionization and MRM models. Results This method showed a good linearity within their respective linear ranges with high correlation coefficients (r2≥0.997) of 4 trichothecenes, and the detection limits for them were ranged from 5 to 20 μg/kg, the average recoveries in the above 3 matrices spike at 3 levels were between 66.9% to 101.8%, with a relative standard deviation (RSD) were in the range from 3.7% to 13.9%. Conclusion This analytical method can meets the requirements for trace assays. In addition, it is simple, rapid, accurate and suitable for the simultaneous determination of 4 kinds of trichothecenes in cookies.

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