摘要
建立了花生样品中4种黄曲霉毒素(黄曲霉毒素B_1、黄曲霉毒素B_2、黄曲霉毒素G_1、黄曲霉毒素G_2)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 C_(18)硅胶混合体系净化后进行检测。采用Hypersil Gold C_(18)柱(100 mm×2.1 mm,1.9μm)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(r^2)均大于0.996,方法定量下限为0.25～1.0μg/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。
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 MgSO 4,100 mg PSA and 400 mg C 18 .The analytes were separated on a Hypersil Gold C 18 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 ( r ^2 )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.
作者
胡巧茹
丛中笑
沙美兰
曹鹏
梁君妮
李晓玉
关丽丽
谢爽
HU Qiao-ru;CONG Zhong-xiao;SHA Mei-lan;CAO Peng;LIANG Jun-ni;LI Xiao-yu;GUAN Li-li;XIE Shuang(Technology Center of Yantai Entry-Exit Inspection and Quarantine Bureau,Yantai264000,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2019年第4期396-402,共7页
Journal of Instrumental Analysis
基金
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)
关键词
高分辨质谱
花生
黄曲霉毒素
农药残留
high resolution mass spectrometry (HRMS )
peanut
aflatoxins
pesticide residues
