固相萃取/超高效液相色谱-串联质谱法测定白术中井冈霉素和丙环唑残留量

Determination of jingangmycin and propiconazole in Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry

建立固相萃取/超高效液相色谱-串联质谱(SPE/UPLC-MS/MS)检测白术鲜样及干样中井冈霉素和丙环唑残留的分析方法。样品经甲醇/水(9∶1,V/V)提取,Oasis HLB和Cleanert AQ C18固相萃取小柱净化,HSS T3超高效液相色谱柱进行分离,电喷雾正离子多重反应监测(MRM)模式进行测定。结果表明:浓度在0.0001~0.1 mg·L^(-1)范围内,井冈霉素和丙环唑在溶剂及基质中的峰面积与其对应的质量浓度间线性关系良好,R^(2)≥0.9996。在添加0.01、0.5、5.0 mg·kg^(-1)标准品浓度下,井冈霉素在白术中的添加回收率为72.4%~85.8%,相对标准偏差(RSD)为0.89%~6.20%;在添加0.005、0.1、1.0 mg·kg^(-1)标准品浓度下,丙环唑在白术中的添加回收率为88.1%~98.9%,RSD为1.4%~4.8%。井冈霉素和丙环唑在白术中的定量限(LOQ)分别为0.01 mg·kg^(-1)和0.005 mg·kg^(-1)。通过对实际样品的检测,表明该方法操作简单,重复性好,准确度、精密度及检出限均可满足农药残留分析要求。

A simple and sensitive method was developed for the determination of jingangmycin A and propiconazole in fresh and dry samples of Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry(SPE/UPLC-MS/MS).The samples were extracted with methanol/water(9∶1,V/V),purified with an Oasis HLB column(for jingangmycin A)and Cleanert AQ C18 column(for propiconazole),and separated on a HSS T3 column,finally analyzed in multiple reaction monitoring(MRM)mode via positive electrospray ionization(ESI+).Under the optimum condition,the calibration curves for the analyte were linear in the range of 0.0001-0.1 mg·L^(-1),with correlation coefficients(R^(2))not less than 0.9996.At spiked levels of 0.01,0.5 and 5.0 mg·kg^(-1),the recoveries for jingangmycin A in two matrices were in the range of 72.4%-85.8%with relative standard deviations(RSD)of 0.89%-6.20%;At spiked levels of 0.005,0.1 and 1.0 mg·kg^(-1),the recoveries for propiconazole in two matrices were in the range of 88.1%-98.9%with relative standard deviations(RSD)of 1.4%-4.8%.The method was simple,reproducible,accurate,precise and the detection limit could meet the requirements of pesticide residue analysis.