免疫亲和柱全自动净化-超高效液相色谱-串联质谱-全碳标记内标法精确测定粮油中玉米赤霉烯酮

doi:10.7506/spkx1002-6630-20190927-339

食品科学 ›› 2020, Vol. 41 ›› Issue (24): 267-272.doi: 10.7506/spkx1002-6630-20190927-339

免疫亲和柱全自动净化-超高效液相色谱-串联质谱-全碳标记内标法精确测定粮油中玉米赤霉烯酮

吴宇，叶金，李丽，李森，轩志宏，崔华，刘洪美，王松雪，马海华，张峰，何建洪

（1.国家粮食和物资储备局科学研究院粮油质量安全研究所，北京 102629；2.河南工业大学信息科学与工程学院，河南郑州 450001；3.睿科仪器（厦门）有限公司，福建厦门 361000）

出版日期:2020-12-25 发布日期:2020-12-28
基金资助:
“十三五”国家重点研发计划重点专项（2016YFE0113000）；中央级公益性科研院所基本科研业务费专项（ZX1922）；中国科协青年人才托举工程项目（2018QNRC001）；河南省教育厅高等学校重点科研项目（18A510002）

Fully 13C Isotope Labeled Internal Standard for the Accurate Quantification of Zearalenone in Cereals and Oils by Ultra-high Performance Liquid Chromatography-Tandem Triple Quadrupole Mass Spectrometry after Automated Purification with Immunoaffinity Column

WU Yu, YE Jin, LI Li, LI Sen, XUAN Zhihong, CUI Hua, LIU Hongmei, WANG Songxue, MA Haihua, ZHANG Feng, HE Jianhong

(1. Institute of Grain and Oil Quality Safety, Academy of National Food and Strategic Reserves Administration, Beijing 102629, China; 2. College of Information Science and Engineering, Henan University of Technology, Zhengzhou 450001, China; 3. Raykol Instrument Co. Ltd., Xiamen 361000, China)

Online:2020-12-25 Published:2020-12-28

摘要/Abstract

摘要： 建立免疫亲和柱全自动净化-超高效液相色谱-质谱-全碳标记内标法精确测定粮油中的玉米赤霉烯酮的方法。结果表明，内标法测定粮油中玉米赤霉烯酮的检出限为0.33 μg/kg，定量限为1 μg/kg，相关系数为0.999 5，回收率为92.7%～101.3%，相对标准偏差为0.02%～3.74%，测定3 种基体质控样品的结果均在标示值范围内，准确性和精密度明显优于外标定量方法。本方法无需氮吹、可批量自动化处理样品提高工作效率，避免因人员操作导致的结果偏差，可用于大量粮油样品中玉米赤霉烯酮的精准测定。

关键词: 全自动免疫亲和柱净化；超高效液相色谱-串联质谱；内标法；粮油；玉米赤霉烯酮

Abstract: An accurate method for the quantification of zearalenone in cereals and oils was developed by automated purification with immunoaffinity column combined with ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS) using a fully 13C isotope labeled standard. The results showed that the quantification limit (LOQ) and detection limit (LOD) of the internal standard method were 0.33 and 1 μg/kg, respectively, with a correlation coefficient R2 of 0.999 5. The recoveries were 92.7%–101.3% with relative standard deviation (RSD) of 0.02%–3.74%. The results obtained by this method for three quality control samples were within the range of certified values. Its accuracy and precision were better than those of the external standard method. The internal standard method allowed the automated and efficient detection of massive samples without the need for nitrogen gas blowing and could avoid the errors caused by manual operations.

Key words: automated purification with immunoaffinity column; ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry; internal standard method; cereals and oils; zearalenone

中图分类号:

TS207.7

吴宇，叶金，李丽，李森，轩志宏，崔华，刘洪美，王松雪，马海华，张峰，何建洪. 免疫亲和柱全自动净化-超高效液相色谱-串联质谱-全碳标记内标法精确测定粮油中玉米赤霉烯酮[J]. 食品科学, 2020, 41(24): 267-272.

WU Yu, YE Jin, LI Li, LI Sen, XUAN Zhihong, CUI Hua, LIU Hongmei, WANG Songxue, MA Haihua, ZHANG Feng, HE Jianhong. Fully 13C Isotope Labeled Internal Standard for the Accurate Quantification of Zearalenone in Cereals and Oils by Ultra-high Performance Liquid Chromatography-Tandem Triple Quadrupole Mass Spectrometry after Automated Purification with Immunoaffinity Column[J]. FOOD SCIENCE, 2020, 41(24): 267-272.

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免疫亲和柱全自动净化-超高效液相色谱-串联质谱-全碳标记内标法精确测定粮油中玉米赤霉烯酮

Fully 13C Isotope Labeled Internal Standard for the Accurate Quantification of Zearalenone in Cereals and Oils by Ultra-high Performance Liquid Chromatography-Tandem Triple Quadrupole Mass Spectrometry after Automated Purification with Immunoaffinity Column

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