超高效液相色谱-串联质谱法测定氰霜唑及其代谢物在铁皮石斛中的残留

Determination of Cyazofamid and Its Metabolite in Dendrobium Officinale Kimuraet Migo by Ultra Performance LiquidChromatography-Tandem Mass Spectrometry

建立了同时测定铁皮石斛中氰霜唑及其代谢物4-氯-5-(4-甲苯基)-1H-咪唑-2-腈(CCIM)的超高效液相色谱-串联质谱分析方法,并对实际样品中的氰霜唑和CCIM进行了检测。样品采用乙腈提取,提取液经0.1%甲酸溶液稀释定容后进行液相色谱串联质谱分析。色谱柱采用Acquity BEH C18进行色谱分离,流动相为0.1%甲酸溶液-乙腈,梯度洗脱;质谱采用电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式采集数据,基质校准外标法定量。结果表明:氰霜唑和CCIM基质标准溶液在0.0001~0.05 mg·L^(-1)浓度范围内定量离子对峰面积与浓度呈良好的线性关系。在0.010~2.0 mg·kg^(-1)添加水平下,氰霜唑在铁皮石斛中的回收率为81%~106%,CCIM在铁皮石斛中的回收率为82%~107%,且相对标准偏差(RSD)最大为3.8%(n=5),方法的最低检出量为1.0×10^(-12)g,最低检出浓度为0.01 mg·kg^(-1),该分析方法操作简单快速,灵敏度和精密度均符合农药残留检测要求。

A method was established to determine the residue of cyazofamid and its metabolite 4-chloro-5-(4-methylphenyl)-1 H-imidazole-2-carbonitrile(CCIM)by UPLC-MS/MS in Dendrobium Officinale Kimura et Migo.The samples were extracted with acetonitrile and the aqueous phase as inject solution after dilution with 0.1%formic acid solution.The LC-MS/MS analytical conditions were as follows:UPLC BEH C18 column,0.1%formic acid solution and acetonitrile as the mobile phase with gradient elution,positive electrospray ionization(ESI+)mode,multiple reaction monitoring(MRM)acquisition mode,and matrix-matched external standard method as quantitative method.Such method displayed a good linearity in the range of 0.0001 mg·L^(-1)to 0.05 mg·L^(-1)for cyazofamidin and CCIM.Results showed that at fortified levels of 0.010 to 2.0 mg·kg^(-1)of cyazofamidin and CCIM in Dendrobium Officinale Kimura et Migo,the average recoveries were 81%~106%and 82%~107%.The maximum of the coefficient of variation were 3.8%(n=5).The limit of detection was estimated to be 1×10^(-12)g,and the limit of quantification was 0.01 mg·kg^(-1).This method is simple and accurate,and it is suitable for determination and confirmation of cyazofamidin and CCIM in Dendrobium Officinale Kimura et Migo.