超高效液相色谱-串联质谱测定桑葚中醚菌酯残留量

Determination of Kresoxim-methyl Residues in Mulberry by UPLC-MS/MS

[目的]建立了桑葚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)。[方法]桑葚样品经乙腈提取,石墨化炭黑氨基复合柱(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]醚菌酯在0.001~0.20 mg/L质量浓度范围内呈良好的线性关系,相关系数R^2大于0.999,方法检出限为0.25μg/kg,测定下限为0.001 mg/kg。在0.001~0.10 mg/kg范围内,准确度(85.0%~96.0%)、精密度(3.12%~9.53%)和提取回收率(86.47%~99.44%)均满足分析方法要求。[结论]该方法适用于桑葚中醚菌酯的残留检测。

[Aims] The ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） method for analysis of kresoxim-methyl residues in mulberry was developed. [Methods] The kresoxim-methyl residues in mulberry were extracted with acetonitrile, purified with Carbon/NH2 column and with the mixture of methanol and 0.1% formic acid solution as mobile phase, and determined under multiple reaction monitoring（ MRM） mode with positive electrospray ionization（ESI-＋） by external standard method. [Results] The calibration curve was good linear between the peak areas and the concentrations of 0.001-0.20 mg/L, the correlation coefficient R-2 was above 0.999. The limit of detection was 0.25 μg/kg and the limit of quantitation was 0.001 mg/kg. When the content of kresoxim-methyl was0.001-0.10 mg/kg, the accuracy（85.0-96.0%）, precision（3.12-9.53%） and recovery（86.47-99.44%） of this method can meet the requirements of analytical method. [Conclusions] This method was suitable for the determination of kresoxim-methyl residues in mulberry.