【摘要】 应用气相色谱-质谱(GC-MS)联用检测了国产新杀虫剂杀虫双。试样(5 g)经用0.1 mol.L-1HCl提取,并经离心分离除去不溶物。所得澄清试液,用0.1 mol.L-1NaOH溶液调节至pH 9,再用0.1 mol.L-1硫化钠处理,随后用CHCl3萃取,将萃取液蒸至近干用甲醇1 mL定容。此溶液供GC-MS检测。气相色谱分析时用弹性石英毛细管色谱柱(DB1701,30 m×0.25 mm,0.25μm)。质谱测定中SIM模式的特征离子为m/z70,103和149。用不同浓度的杀虫双标准溶液(0.1,0.2,0.5和1.0 mg.L-1)制作标准曲线作为定量依据。用标准加入法进行平行12次测定,得到RSD在8.5%~16.8%之间,回收率在80%~91%之间。更多还原

【Abstract】 Dimehypo,a new Chinese pesticide,in the sample（5 g） was extracted by shaking with 0.1 mol·L^-1 HCl for 30 min,and separated from the insoluble substances by centrifuging.The clear sample solution was adjusted to pH 9 with 0.1 mol·L^-1 NaOH solution,and after treating with 0.1 mol·L^-1 Na₂S,it was extracted with CHCl₃ in a separatory funnel.The CHCl₃ extract was evaporated to near dryness and diluted to 1 mL with methanol.Through the above treatment the pesticide dimehypo was dissociated and a dissociation product called "Shacandusu" was obtained which was further detected and determined by hyphenated GC-MS.Elastic quartze capillary chromatographic column（DB1701,30 m×0.25 mm,0.25 μm） was used in gas chromatography.The characterizing ions of SIM mode were m/z 70,103,149.Standard curve prepared with dimehypo standard solutions of different concentrations(0.1,0.2,0.5,1.0 mg·L^-1) was used in the quantitative analysis.RSD′s（n=12） obtained were in the range of 8.5% to 16.8% and recoveries in the range of 80% to 91%.更多还原