全碳标记稳定同位素内标-超高效液相色谱-串联质谱法测定粮食中16 种真菌毒素

doi:10.7506/spkx1002-6630-201718046

食品科学 ›› 2017, Vol. 38 ›› Issue (18): 297-303.doi: 10.7506/spkx1002-6630-201718046

全碳标记稳定同位素内标-超高效液相色谱-串联质谱法测定粮食中16 种真菌毒素

吴宇，辛媛媛，叶金，张艳，谢刚，李丽，黎睿，王松雪，张婷岚

（1.国家粮食局科学研究院，北京 100037；2.国家粮食局标准质量中心，北京 100036；3.赛默飞世尓科技（中国）有限公司，北京 100007）

出版日期:2017-09-25 发布日期:2017-09-04
基金资助:
“十三五”国家重点研发计划重点专项（2016YFE0113000）；公益性行业（粮食）科研专项（201313005）

Suitability of Fully 13C Isotope Labeled Internal Standards for the Simultaneous Determination of 16 Mycotoxins in Grains by UPLC-MS/MS

WU Yu, XIN Yuanyuan, YE Jin, ZHANG Yan, XIE Gang, LI Li, LI Rui, WANG Songxue, ZHANG Tinglan

(Academy of State Administration of Grain, Beijing 100037, China; 2. Standards and Quality Center of State Administration of Grain, Beijing 100036, China; 3. Thermo Fisher Scientific (China) Co. Ltd., Beijing 100007, China)

Online:2017-09-25 Published:2017-09-04

摘要/Abstract

摘要： 考察高效液相色谱-串联质谱-全碳标记的稳定同位素内标法精确测定小麦和玉米中16?种真菌毒素方法的适用性。样品经提取稀释、加入内标，高效液相色谱-串联质谱测定。结果表明，16?种真菌毒素线性相关系数大于0.997，3?个水平的添加回收率为83%～114.3%，相对标准偏差为0.9%～13%，定量限为0.5～200?μg/kg，通过检测FAPAS04223质控样品和小麦、玉米样品验证了方法的准确性和适用性，能够快速、批量、准确的测定小麦和玉米中16?种真菌毒素，为我国粮食真菌毒素污染监测提供便利。

关键词: 直接提取, 稳定同位素稀释, 高效液相色谱-串联质谱, 真菌毒素, 粮食

Abstract: This work investigated the suitability of applying fully 13C isotope labeled mycotoxins as internal standards for the accurate determination of 16 mycotoxins in maize and wheat by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target analytes in samples were extracted, diluted, and detected by UPLC-MS/MS after addition of internal standards. The results showed that all 16 mycotoxins displayed good linear relationships with correlation coefficients more than 0.997. Recoveries of the analytes were in the range of 83%–114.3% with relative standard deviations of 0.9%–13%. The limits of quantification (LOQs) of the method ranged from 0.5 to 200 μg/kg. Maize reference materials, and corn and wheat samples were analyzed by this method to validate its accuracy and applicability. The method could accurately, quickly detect 16 mycotoxins in grains in batch.

Key words: direct dilution, stable isotope dilution, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), mycotoxins, grains

中图分类号:

TS207.3

吴宇，辛媛媛，叶金，张艳，谢刚，李丽，黎睿，王松雪，张婷岚. 全碳标记稳定同位素内标-超高效液相色谱-串联质谱法测定粮食中16 种真菌毒素[J]. 食品科学, 2017, 38(18): 297-303.

WU Yu, XIN Yuanyuan, YE Jin, ZHANG Yan, XIE Gang, LI Li, LI Rui, WANG Songxue, ZHANG Tinglan. Suitability of Fully 13C Isotope Labeled Internal Standards for the Simultaneous Determination of 16 Mycotoxins in Grains by UPLC-MS/MS[J]. FOOD SCIENCE, 2017, 38(18): 297-303.

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全碳标记稳定同位素内标-超高效液相色谱-串联质谱法测定粮食中16 种真菌毒素

Suitability of Fully 13C Isotope Labeled Internal Standards for the Simultaneous Determination of 16 Mycotoxins in Grains by UPLC-MS/MS

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