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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。
Gas chromatography-mass spectrometry (GC-MS) combined detection of domestic new pesticides insecticidal double. The sample (5 g) was extracted with 0.1 mol·L-1HCl and centrifuged to remove insolubles. The resulting clear test solution was adjusted to pH 9 with 0.1 mol. L-1 NaOH solution, treated with 0.1 mol. L-1 sodium sulfide, and then extracted with CHCl3. The extract was evaporated to near dryness with 1 mL of methanol. This solution is for GC-MS detection. Gas chromatographic analysis was performed on a flexible quartz capillary column (DB1701, 30 m × 0.25 mm, 0.25 μm). The characteristic ions for SIM mode in mass spectrometry were m / z 70, 103 and 149. The calibration curves were prepared by using different concentrations of insecticidal double standard solution (0.1, 0.2, 0.5 and 1.0 mg.L-1) as the quantitative basis. The standard addition method for parallel determination of 12 times, the RSD was 8.5% to 16.8%, the recovery was between 80% to 91%.