摘要
建立了超高效液相色谱-串联质谱法(High Performance Liquid Chromatography-tandem Mass Spectrometry,HPLC-MS/MS)测定大豆中吡虫啉残留量的检测方法。样品经过乙腈提取、QuECHERS(Quick、Easy、Cheap、Effective、Rugged、Safe)法除去杂质,氮吹复溶后,采用InfinityLab Poroshell 120 EC-C_(18)(2.1×100 mm×1.9μm)色谱柱分离,以乙腈和0.1%甲酸水为流动相梯度洗脱,采用多反应检测方式和正离子扫描方式检测,以外标法定量。结果表明,吡虫啉在5.317~170.144 ng/mL范围内有良好的线性关系,相关系数为0.9995;检出限为3.0μg/kg,定量限为10.0μg/kg;在10,50,100μg/kg这3个加标水平回收率为88.6%~102.3%,相对标准偏差(RSD)为1.1%~2.3%。该方法操作简便、灵敏度高、重现性好,适用于豆类中吡虫啉残留量的测定。
A High Performance Liquid chromatography-tandem Mass Spectrometry(HPLC-MS/MS)method was developed for the determination of imidacloprid residues in soybean.The sample was extracted with acetonitrile,purified with QuECHERS method,Nitrogen blow and dissolved,and separated on an Infinity Lab Poroshell 120 EC-C_(18)(2.1×100 mm,1.9μm)column,acetonitrile and 0.1%formic acid water were used as mobile phase for gradient elution.Multiple reaction detection method and positive ion scanning method were used for detection.The quantitative analysis was performed by external standard method.The results showed that imidacloprid had good linear relationships in the range of 5.317~170.144 ng/mL,and the correlation coefficients were all greater than 0.9995;the limit of detection was 3.0μg/kg,and the limit of quantification was 10.0μg/kg;the recovery rate of at the spiked levels of 10,50 and 100μg/kg was 88.6%~102.3%,and the relative standard deviations(RSD)was 1.1%~2.3%.The method was simple,sensitive and reproducible.It was suitable for the determination of imidacloprid residues in soybean.
作者
罗长琴
朱显平
邹璇
吴秋杰
黄小兰
谭春蓉
LUO Changqin;ZHU Xianping;ZOU Xuan;WU Qiujie;HUANG Xiaolan;TAN Chunrong(Chongqing Wanzhou Institute for Food and Drug Inspection,Chongqing 404100,China;Chongqing Vocational Institute of Safety&Technoligy,Chongqing 404100,China;Chayuan Xincheng Middle School,Chongqing 401336,China)
出处
《农产品加工》
2022年第22期62-64,共3页
Farm Products Processing