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超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定花生中4种黄曲霉毒素和11种农药残留
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胡巧茹,丛中笑,沙美兰,曹鹏,梁君妮,李晓玉,关丽丽,谢爽 烟台出入境检验检疫局检验检疫技术中心 
基金项目:山东检验检疫局科研计划项目(SK201712);国家重点研发计划“国家质量基础的共性技术研究与应用”重点专项(2017YFF0211100)
中文摘要:建立了花生样品中4种黄曲霉毒素(黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2)和11种农药残留(啶虫脒、乙草胺、多菌灵、克百威、毒死蜱、苯醚甲环唑、烯酰吗啉、吡虫啉、嘧霉胺、戊唑醇、噻虫嗪)的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UPLC-HRMS)。样品经乙腈-水-乙酸提取液(84∶15∶1,体积比)提取,1.0 g硫酸镁、100 mg PSA与400 mg C18硅胶混合体系净化后进行检测。采用Hypersil Gold C18柱(100 mm×2.1 mm,1.9 μm)分离,用UPLC-HRMS进行检测。结果显示,4种黄曲霉毒素和11种农药残留在各自的质量浓度范围内线性关系良好,相关系数(r2)均大于0.996,方法定量下限为0.25~1.0 μg/kg,样品的加标回收率为79.4%~120%,相对标准偏差(RSD,n=6)为4.2%~10%。该方法的灵敏度高、结果准确、可靠,能够实现对花生样品中4种黄曲霉毒素和11种农药残留含量的同时检测。
中文关键词:高分辨质谱  花生  黄曲霉毒素  农药残留
 
Determination of 4 Aflatoxins and 11 Pesticide Residues in Peanut by Ultrahigh Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
Abstract:A method was developed for the determination of 4 aflatoxins and 11 pesticide residues in peanut by ultrahigh performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-HRMS).The samples were extracted with acetonitrile-water-acetic acid(84∶15∶1,by volume),and the extracts were cleaned up with 1.0 g MgSO4,100 mg PSA and 400 mg C18.The analytes were separated on a Hypersil Gold C18 column(100 mm×2.1 mm,1.9 μm),and quantified by UPLC-HRMS.Results showed that 4 aflatoxins and 11 pesticide residues had good linear relationships in their respective mass concentration ranges with their correlation coefficients(r2)more than 0.996.The limits of quantitation(LOQs)of the method ranged from 0.25 μg/kg to 1.0 μg/kg.The spiked recoveries for 4 aflatoxins and 11 pesticide residues at three spiked levels ranged from 79.4%to 120%with relative standard deviations(RSD,n=6) of 4.2%-10%.With the advantages of high sensitivity and reliability,the method was suitable for the simultaneous determination of 4 aflatoxins and 11 pesticide residues in peanut.
Key Words:high resolution mass spectrometry(HRMS)  peanut  aflatoxins  pesticide residues
引用本文:胡巧茹,丛中笑,沙美兰,曹鹏,梁君妮,李晓玉,关丽丽,谢爽.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定花生中4种黄曲霉毒素和11种农药残留[J].分析测试学报,2019,(4):396-402.
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