高效液相色谱-串联质谱检测高粱中喹草酮残留量

[目的]建立了高效液相色谱-串联质谱(HPLC-MS/MS)快速检测高粱和秸秆中喹草酮残留的分析方法。[方法]样品经乙腈提取,C18吸附剂净化,多反应监测模式检测,基质匹配标准品外标法定量。[结果]在0.01～5mg/L范围内,喹草酮在高粱等基质中的质量浓度与对应的峰面积间呈良好的线性关系,其相关系数均大于0.9992。在0.02～2 mg/kg添加水平下,喹草酮在高粱和秸秆中的平均回收率为86%～102%,相对标准偏差(RSD)为2%～19%。喹草酮在高粱和秸秆中的定量限(LOQ)均为0.02 mg/kg。[结论]该方法简便、快速、准确,可用于高粱中喹草酮的残留检测。

Analysis of Quinotrione Residues in Sorghum by HPLC-MS/MS

[Aims] A rapid and sensitive analytical method for the determination of quinotrione residues in sorghum and straw was established based on high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).[Methods] The samples were extracted with acetonitrile and purified with octadecylsilane(C18). The mass spectrometer was performed under multi-reaction monitoring mode. The quinotrione residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect. [Results] The calibration curves for quinotrione were linear in the range of 0.01-5 mg/L with correlation coefficients of more than 0.9992. When the addition level ranged from 0.02 to 2 mg/kg, the average recoveries of quinotrione in sorghum and straw were 86-102%,and the relative standard deviation(RSD) ranged from 2 to 19%. The limit of quantitation(LOQ) was 0.02 mg/kg in different matrices. [Conclusions] This method is simple, rapid and accurate, and can be adapted for the confirmation of quinotrione residues in sorghum samples.