UPLC-MS/MS同时测定“壮根灵”类农肥中18种植物生长调节剂的含量

Simultaneous Determination of Contents of 18 Plant Growth Regulators in Agricultural Fertilizer of“Zhuanggenling”by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定“壮根灵”类农肥中18种植物生长调节剂的含量。样品经1%醋酸乙腈提取后,采用UPLC-MS/MS进行测定。色谱柱:Waters Acquity UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm);流动相:0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱;流速:0.3 mL/min;柱温:20℃;多反应监测(MRM)模式。结果表明,18种植物生长调节剂线性关系良好,线性范围为2~300μg/L(r≥0.997),检出限为0.09~2.51μg/g,定量限为0.22~7.69μg/g,精密度RSD均小于9%,平均加样回收率为85.4%~95.3%,RSD为2.6%~8.1%(n=9)。采用该法对10批次“壮根灵”类农肥中植物生长调节剂含量进行了检测,含量为0.19~122.60 mg/g。该方法前处理简单、灵敏度高、准确快速,可用于“壮根灵”类农肥中植物生长调节剂的定性和定量分析。

To establish an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of contents of 18 plant growth regulators(PGRs)in agricultural fertilizer of“Zhuanggenling”.Samples were extracted with 1%acetonitrile acetic acid,and then determined by UPLC-MS/MS with a Waters Acquity UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm)chromatographic column,the mobile phase consisted of 0.1%formic acid solution(A)and acetonitrile(B)for gradient elution at a flow rate of 0.3 mL/min at the column temperature of 20℃using multiple reaction monitoring(MRM)mode.The result showed that the linear range of 18 PGRs were 2~300μg/L with r no less than 0.997.The detection and quantitative limits were 0.09~2.51μg/g and 0.22~7.69μg/g,respectively with the RSDs of precision less than 9%.Average recovery was 85.4%~95.3%with RSD 2.6%~8.1%(n=9).The contents of 18 PGRs in 10 batches of agricultural fertilizer of“Zhuanggenling”were 0.19~122.60 mg/g.The method proved a simple pre-treatment,rapid,sensitive,accurate,and suitable way for the simultaneous qualitative and quantitative determination of 18 PGRs contents in agricultural fertilizer of“Zhuanggenling”.