超高效液相色谱-串联质谱法同时测定党参中18种植物生长调节剂残留量

Simultaneous determination of 18 plant growth regulator residues in Codonopsis Radix by ultra performance liquid chromatography-tandem mass spectrometry

采用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了同时测定党参中18种植物生长调节剂残留量的分析方法。采用Waters Acquity UPLC BEH C18色谱柱;流动相:0.1%甲酸水溶液-乙腈,梯度洗脱;流速:0.1mL/min;柱温:20℃;电喷雾多反应监测模式。样品以乙腈直接提取后经QuEChERS法净化,采用UPLC-MS/MS分析,用空白基质匹配标液外标法定量。结果表明,18种植物生长调节剂在各自浓度范围内线性良好,相关系数均大于0.995,检出限为0.06~4.50μg/kg,定量限为0.21~15.5μg/kg,RSD均小于10%,平均加样回收率为76.2%~100.8%,RSD为3.5%~8.5%。对76批次党参中植物生长调节剂残留情况进行了筛查。方法可用于党参中植物生长调节剂残留的定性和定量分析。

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous determination of 18 plant growth regulator(PGR)residues in Codonopsis Radix.The chromatographic column was Waters Acquity UPLC BEH C18;the mobile phase consisted of 0.1%formic acid solution and acetonitrile for gradient elution with the flow rate of 0.1 m L/min;the column temperature was20℃,and multiple reaction monitoring(MRM)mode was used for MS detection.Samples were extracted with acetonitrile,and then determined by UPLC-MS/MS directly after Qu EChERS clean up.The matrix-matched external standard method was used for quantitative analysis.The calibration curves of 18 PGRs showed good linearity with correlation coefficients higher than 0.995.The quantitative limits were 0.21-15.52μg/kg,the detection limits were 0.06-4.50μg/kg;the RSDs were less than 10%;and the average recoveries were76.2%-100.8%with the RSD of 3.5%-8.5%.The PGR residues in 76 batches of Codonopsis Radix were analyzed by this method.The method is suitable for the simultaneous determination of 18 PGR residues in Codonopsis Radix.