桑葚中克百威和3-羟基克百威残留量测定

摘要

An ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) assay for quantification of carbofuran and 3-hydroxycarbofuran, in mulberry was developed. The carbofuran and 3-hydroxycarbofuran were extracted by acetonitrile,purified by Carbon/NH2and analyzed with a methanol-0.1% formic acid solution-acetonitrile mobile phase. The residues of carbofuran and 3-hydroxycarbofuran were determined by multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+),and quantified by the method of external standard. The results showed that the calibration curves were good linear relationship between the ratio of the peak areas and the concentrations of from 1.00 to 200μg/L and the correlation coefficient(R2)was both more than 0.99.The limits of detection were 0.25 μg/kg and the limit of quantification were 1.00 μg/kg. The recovery, precision and matrix effect of this method, with 1.00-100 μg/kg additive amount, can meet the requirements of analytical method. This method was suitable for the determination of carbofuran and 3-hydroxycarbofuran residues in mulberry.%建立了桑葚中克百威和3-羟基克百威残留检测的超高效液相色谱-串联质谱方法(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS).桑葚样品经乙腈提取,石墨化碳黑氨基复合柱(Carbon/NH2)净化,以甲醇和0.1%甲酸水溶液作为流动相洗脱,采用电喷雾离子源正离子模式(ESI+),多反应监测(MRM)方式进行采集,外标法定量.结果表明,克百威和3-羟基克百威在1.00~200.00 μg/L浓度范围内呈现良好的线性关系,相关系数(R2)均大于0.99,方法检出限均为0.25 μg/kg,定量限均为1.00 μg/kg.在1.00~100.00 μg/kg添加浓度范围内,回收率、精密度和基质效应均满足分析方法要求.该试验方法适用于桑葚中克百威和3-羟基克百威残留量的测定.