QuEChERS-LC-MS/MS法测定干制红枣中多菌灵的残留量  

Determination of Carbendazim Residues in Dry-cure Red Jujube by QuEChERS-Liquid Chromatography-Tandem Mass Spectrometry

作　　者：曾敏 杨晋青[2] 俞晓琴 陈慧 Zeng Min;Yang Jinqing;Yu Xiaoqin;Chen Hui(Zhejiang Wufangzhai Industrial Co.,LTD.;Shanghai Institute of Quality Inspection and Technical Research)

机构地区：[1]浙江五芳斋实业股份有限公司 [2]上海市质量监督检验技术研究院

出　　处：《中国质量与标准导报》2022年第4期67-72,共6页China Quality and Standards Review

摘　　要：建立运用QuEChERS-液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定干制红枣中多菌灵残留量的分析方法。样本中的多菌灵采用乙腈超声萃取法和QuEChERS法进行净化,净化液通过0.22 μm滤膜过滤后,采用LC-MS/MS测定。经 色谱柱Waters Atlantis T3 C18(3 μm,2.1 mm×100 mm)净化分离后,经电喷雾离子源(ESI源)电离子化、正离子扫描和多化学反应监测模式检验,并使用基质对应的标准曲线外标法定量分析。多菌灵在2.5 ng/mL~100 ng/mL的标准质量浓度范围内呈正常线性关系,相关系数为0.9965。在10.0 μg/kg、20.0 μg/kg和100 μg/kg三个不同添加梯度的平均回收率为86.9%~109.1%,RSD (n=6)为3.01%~7.27%。多菌灵的方法定量限为10.0 μg/kg。该方法具备高准确性、高灵敏度、良好再现性等优点,并能达到对干枣中多菌灵的残留测定要求。In this study,a rapid,highly sensitive and selective method was developed for the simultaneous determination of residues of Carbendazim Residues in dry-cure red jujube by liquid chromatography-tandem mass spectrometry (LC-MS/MS).Carbendazim is extracted from the samples with acetonitrile,cleaned up by QuEChERS method.After filtered with a 0.22 μm membrane the resulting samples determined by LC-MS /MS performing on positive electrospray ionization and the multiple reactions monitoring mode (MRM).The matrix-matched external standard calibration curves were used for quantitative analysis.The linearly dependent coefficient of Carbendazim is 0.9965 in the concentration range of 2.5 ng/mL~100 ng/mL.The added recoveries were between 86.9%~109.1% with the concentration levels at 10.0 μg/kg、20.0 μg/kg and 100 μg/kg for Carbendazim.RSD (n=6) were in the range of 3.01%~7.27%.The limit of quantifiation (LOQ) is 10.0 μg/kg.With the advantages of efficient,accurate,high sensitivity and good reproducibility,the method is suitable for the determination of carbendazim in dry-cure red jujube.

关 键 词：QUECHERS 液相色谱-串联质谱法 多菌灵 干制红枣 

分 类 号：R28[医药卫生—中药学]