亲水作用液相色谱串联质谱法测定土壤中春雷霉素含量

Determination of Kasugamycin in Brown Rice with HILIC-MS/MS

【目的】建立土壤中春雷霉素含量的亲水作用色谱质谱联用测定方法。【方法】样品用甲醇-水（体积比9：11溶液提取，经HLB和SCX固相萃取小柱净化，以WatersHPLCBEHHILIC色谱柱分离，采用UPLC—MS／MS多反应监测（MRM）iE离子模式测定，外标法定量。【结果】春雷霉素检出限为0．005mg／kg。0．005、0．05、0．1mg／kg三个质量分数添加水平，回收率为74．0％-85．7％，相对标准偏差为5．1％-9．0％佃=5）。【结论】该方法的灵敏度和精密度满足残留分析的要求，适合大批样品的检测。

[Aims] A method of determination for Kasugamycin in soil by HILIC-MS/MS was described. [Methods] The analytes were extracted from samples using methanol and water （9 ： 1, by vol）, and purified by HLB and SCX solid phase extraction column, then analyzed using UPLC-MS/MS in selective reaction monitoring （MRM） mode via positive electrospray ionization with a Waters HPLC BEH HILIC column as the analytical column. All the analytes were quantified by the external standard. [Results] The limits of detection was 0.005 mg/kg. The results from the test of three concentration levels （every level reapeated five times） showed that the overall recoveries were between 74.0 and 85.7%, and the RSD value were 5.1-9.0%（n=5）. [Conclusions] The method had high sensitivity, accuracy and was suitable for the detection of large numbers of samples.