马蹄金中10种真菌毒素UPLC-MS/MS检测方法的建立  

Establishment of UPLC-MS/MS determination of 10 mycotoxins in Dichondra micrantha Ulb.

作　　者：覃冬杰 丘莹 王宏虹 李萍 黄惠琳 QIN Dong-jie;QIU Ying;WANG Hong-hong;LI Ping;HUANG Hui-lin(Liuzhou Quality Inspection and Testing Research Center,Liuzhou 545006,China;Liuzhou Hospital,Guangzhou Women and Children's Medical Center,Liuzhou 545616,China;Guangxi-Asean Food Inspection Center,Nanning 530022,China)

机构地区：[1]柳州市质量检验检测研究中心,广西柳州545006 [2]广州市妇女儿童医疗中心柳州医院,广西柳州545616 [3]广西-东盟食品检验检测中心,广西南宁530022

出　　处：《西南民族大学学报（自然科学版）》2023年第5期530-536,共7页Journal of Southwest Minzu University(Natural Science Edition)

基　　金：广西壮族自治区中医药管理局自筹科研课题(GXZYZ20210118)。

摘　　要：建立马蹄金中10种真菌毒素的测定方法.基于QuEChERS法对样品进行前处理,应用UPLC-MS/MS法进行样品检测,色谱柱:Boltimate C_(18)(2.1×100 mm,2.6μm);流动相:0.1%甲酸溶液(A)-乙腈(B),梯度洗脱;流速:0.3 mL/min;进样量:1μL;电离模式:正、负离子同时电离;监测采集模式:MRM(多反应监测模式);定量分析方法:基质标准曲线法.结果表明,在各自浓度范围内,10种真菌毒素均有良好线性关系,10种真菌毒素检出限为(0.2~13.6μg/kg),定量限为(0.7~45.3μg/kg),回收率为82.5%~109.2%,RSD为1.1%~5.8%.不同来源的样品中真菌毒素检出率为70%,污染值范围分别为AFB1(0.8~3.9μg/kg)、AFG1(0.9μg/kg)、OTA(2.0~7.5μg/kg)、ZEN(11.6~58.7μg/kg)、FB1(28.6~43.0μg/kg)、DON(79.4~139.3μg/kg).该方法操作简便、快速、准确、灵敏度高,适用于马蹄金中10种真菌毒素的快速测定.To establish a method for determination of 10 mycotoxins in D.micrantha Ulb.,the samples were pretreated by QuEChERS method and determined by UPLC-MS/MS on Boltimate C_(18)(2.1×100 mm,2.6 μm)with mobile phase of 0.1% formic acid-acetonitrile.The flow rate was 0.3 mL/min and injection volume was 1 μL.ESI source was applied and operated in positive and negative ion mode,the multi-reaction monitoring mode was used to quantitative analysis with matrix-matched calibration curves.The results showed that 10 kinds of mycotoxins had a good linear relationship in the concentration ranges,the limits of detection were 0.2-13.6 μg/kg and limits of quantitation were 0.7-45.3 μg/kg,the recoveries were 82.5%-109.2%,and RSDs were 1.1%-5.8%.The positive rate of mycotoxins in the samples was 70% and the ranges of contamination values were AFB_1(0.8-3.9 μg/kg),AFG_1(0.9μg/kg),OTA(2.0-7.5 μg/kg),ZEN(11.6-58.7 μg/kg),FB_1(28.6-43.0 μg/kg),DON(79.4-139.3 μg/kg).The method was simple,fast,accurate and high sensitive,suitable for determination of 10 mycotoxins in D.micrantha Ulb.D.micrantha Ulb.contaminated with mycotoxins which had security risks,and monitoring of planting and storage should be strengthened.

关 键 词：QUECHERS UPLC-MS/MS 马蹄金 真菌毒素 

分 类 号：R954[医药卫生—药学]