超高效液相色谱-串联质谱方法测定桑葚中吡虫啉和啶虫脒残留量

Determination of Imidacloprid and Acetamiprid Residue in Mulberry by UPLC-MS/MS

建立了桑葚中吡虫啉和啶虫脒残留检测的超高效液相色谱-串联质谱方法(UPLC-MS/MS)。桑葚样品经乙腈提取,石墨化碳黑氨基复合柱(Carbon/NH_2)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,该试验方法简单,灵敏,选择性好,精密度高,啶虫脒和吡虫啉在0.10~100μg/L浓度范围内呈现良好的线性关系,相关系数R^2>0.99,方法检出限为0.02μg/kg,测定下限为0.10μg/kg。在1.00~100μg/kg添加浓度范围内,回收率、精密度均满足分析方法要求。

An ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）method for quantifying of imidacloprid and acetamiprid residue in mulberry was developed.The samples were firstly extracted by acetonitrile and purified by Carbon/NH2,then eluted with mobile phase of methanol-0.1 %,formic acid solution-acetonitrile.The residues of imidacloprid and acetamiprid were determined by multiple reaction monitoring（MRM）mode with positive electrospray ionization（ESI^＋）and external standard method.The results showed that this method was simple,sensitive and with good selectivity and high precision.The calibration curve was good linear at the concentrations range of 0.10 to 100μg/L with the correlation coefficient R^2〉0.99.The limit of detection of the method was 0.02μg/kg and the limit of quantitation was 0.10μg/kg.The recovery,accuracy and precision of this method,at the fortified level of 1.00-100μg/kg,was applicable of residue analysis.