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目的建立以同位素为内标物同时测定水果中7种农药残留(多菌灵、甲基硫菌灵、甲霜灵、嘧霉胺、三唑酮、氯吡脲、2,4-二氯苯氧乙酸)的超高效液相色谱-串联质谱(UPLC/MS/MS)方法。方法样品经1%(V/V)乙酸的乙腈溶液提取,无水硫酸镁和醋酸钠脱水,分散固相萃取管净化,ACQUITY HSS T3色谱柱分离,以乙腈-5mmol/L甲酸铵10mmol/L甲酸溶液为流动相,流速0.3mL/min,柱温30℃,电喷雾电离,正负离子分段扫描和多反应监测模式检测,同位素内标法定量。结果 7种农药在10~200μg/kg范围内线性关系良好。平均回收率73.1%~103%,RSD=2.1%~5.0%。检出限(LOD)为0.25~0.65μg/kg,定量限(LOQ)为0.83~2.16μg/kg。结论该方法简便快速,定量准确,可满足多种水果中7种农药残留的检测要求。
Objective To establish a method for the simultaneous determination of seven kinds of pesticide residues in fruits by using isotope as internal standard (carbendazim, thiophanate-methyl, metalaxyl, pyrimethanil, triadimefon, clopidamide, 2,4-dichlorobenzene Oxyacetic acid) by ultra performance liquid chromatography-tandem mass spectrometry (UPLC / MS / MS) method. Methods The samples were extracted with 1% (v / v) acetic acid in acetonitrile, dehydrated with anhydrous magnesium sulfate and sodium acetate, and purified by dispersive solid-phase extraction tubes. The separated samples were separated on an ACQUITY HSS T3 column with acetonitrile-5 mmol / L ammonium formate 10 mmol / The formic acid solution was used as the mobile phase at a flow rate of 0.3 mL / min, column temperature of 30 ℃, electrospray ionization, positive and negative ion scanning and multi-reaction monitoring mode, and isotope internal standard method. Results Seven kinds of pesticides showed good linearity in the range of 10 ~ 200 μg / kg. The average recovery 73.1% ~ 103%, RSD = 2.1% ~ 5.0%. The limit of detection (LOD) was 0.25 ~ 0.65μg / kg, and the limit of quantification (LOQ) was 0.83 ~ 2.16μg / kg. Conclusion The method is simple, rapid and accurate. It can meet the detection requirements of seven kinds of pesticide residues in a variety of fruits.