分散固相萃取-气相色谱-串联质谱法同时测定稻谷中三种烯虫酯类保幼激素类似物残留

Simultaneous determination of three methoprene juvenile hormone analogues in paddy by dispersive solid-phase extraction combined with gas chromatography-mass spectrometry

以分散固相萃取(DSPE)作为样品前处理手段,采用气相色谱-串联质谱(GC-MS/MS)检测技术,建立了适用于稻谷中3种烯虫酯类保幼激素类似物残留量同时测定的方法。样品使用1%乙酸-乙腈提取,经1.2 g无水硫酸镁、0.4 g N-丙基乙二胺(PSA)、0.2 g十八烷基硅烷键合硅胶(C18)分散萃取净化,采用DB-1 701(30 m×0.25 mm,0.25μm)毛细管柱分离,动态多重反应监测模式下(DMRM)测定,基质匹配标准曲线内标法定量。结果表明,3种保幼激素类似物在0.01~0.32 mg/L质量浓度范围内线性关系良好,相关系数均大于0.999,烯虫乙酯定量限为0.005 mg/kg,烯虫炔酯和烯虫酯定量限为0.01 mg/kg,3个添加水平(0.02,0.1,0.2 mg/kg)回收率分别在86.0%~107.3%之间,相对标准偏差为1.0%~5.7%(RSDs,n=6)。应用该方法对市售25份稻谷样品进行检测,3种保幼激素类似物均未检出。该方法具有操作简便、灵敏度高,准确度好等优点,适用于稻谷中3种烯虫酯类保幼激素类似物残留量的同时测定。

An effective method was developed for the determination of three methoprene juvenile hormone analogues in paddy by dispersive solid-phase extraction combined with gas chromatography-tandem mass spectrometry.The target compounds were extracted with 1%(v/v)acetic acid-acetonitrile,and purified by 1.2 g MgSO4,0.4 g primary secondary amine(PSA)and 0.2 g C18.After separation on a DB-1701(30 m×0.25 mm×0.25 μm) column,the analytes were detected by GC-MS/MS in the dynamic multiple reaction monitoring(DMRM)mode and quantified using theMatrix matching standard curve internal standard method.Good linearities were obtained for the three methoprene juvenile hormone analogues in the linear range of 0.01-0.32 mg/L,with correlation coefficients larger than 0.999,The limits of quantitation(LOQs) were 0.005-0.01mg/kg.The average recoveries at three levels of 0.02,0.1,0.2 mg/kg ranged from 86.0% to 107.3%,respectively.The relative standard deviations(RSDs,n=6) ranged from 1.0% to 5.7%.25 samples sold in the market were detected,three juvenile hormone analogues were not detected in all the samples.However,this method has certain advantageous such as simple operation,high sensitivity,and good accuracy.In conclusion,this method is suitable for the simultaneous determination of the three methoprene juvenile hormone analogues in paddy.