超高效液相色谱-串联质谱测定草莓中醚菌醋残留量

Determination of Kresoxim-methyl Residue in Strawberry by UPLC-MS/MS

建立了草莓中醚菌酯残留检测的超高效液相色谱-串联质谱方法(UPLC-MS/MS)。草莓样品经乙腈提取,石墨化碳黑氨基复合柱(ProElut CARB/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,醚菌酯在0.50～50.00μg/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0.10μg/kg,测定下限为0.50μg/kg。在0.50～50.00μg/kg范围内,回收率(92.2%～95. 4%)、精密度(2.57%～5.34%)和提取回收率(92. 19%～95. 41%)均满足分析方法要求。

An ultra performance liquid chromatography tandem mass spectrometry （UPLC -MS/ MS） assay was developed for quantification of kresoxim - methyl residue in strawberry. The sample was extracted by acetonitrile, purified by ProElut CARB/NH2, eluted with a methanol -0. 1% for- mic acid solution - acetonitrile as mobile phase. The residues of kresoxim - methyl were determined by multiple reaction monitoring （ MRM ） mode with positive electrospray ionization （ ESI^＋ ） and quantified by external standard method. The results showed that this method was simple, sensitive, selective and highly precise, kresoximmethyl showed a good linear relationship in the concentra- tion range of 0. 50 -50. 00μg/L, the correlation coefficient R^2 〉 0. 99. The limit of detection of the method was 0. 10μg/kg and the limit of quantitation was 0. 50μg/kg. The accuracy （92.2% - 95.4% ）, precision （2. 57% -5.34% ） and recovery （92. 19% -95.41% ） , at the spiked level of 0. 50 -50. 001μg/kg, all meet the requirements of analytical method.