杀虫涂料中拟除虫菊酯类化合物的气相色谱-质谱检测方法

Test of Pyrethroid Compounds in Insecticidal Coatings by the Method of Gas Chromatography-Mass Spectrometry (GC-MS)

建立了杀虫涂料中6种拟除虫菊酯类杀虫剂(丙烯菊酯、苄呋菊酯、胺菊酯、氯菊酯、氯氰菊酯、溴氰菊酯)的气相色谱-质谱检测方法,系统研究了丙酮、正己烷、乙腈等有机溶剂对6种拟除虫菊酯类杀虫剂的提取效率,优化了样品前处理过程和色谱分析条件。样品经无水硫酸钠进行脱水后,用V(丙酮)∶V(正己烷)=1∶1的混合溶剂进行提取,提取液用有机膜过滤,用GC-MS进行测定,6种菊酯杀虫剂在10～100mg/L的浓度范围内线性关系良好,相关系数大于0.99。以市场上普遍销售的水性清漆和水性木器涂料进行了加标回收试验,结果表明:本方法的回收率范围为80.0%～99.6%,方法的相对标准偏差(RSD)小于5.0%,方法检出限为0.38～1.96mg/L。本方法简便、快速、灵敏、精密度好,获得满意结果。

Gas Chromatography-Mass Spectrometry method for 6 insecticides, allethrin, resmethrin, tetramethrin, permethrin, cypermethrin and deltamethrin, is established. This paper studies the extraction efficiency of the 6 insecticides respectively by acetone, n-hexane and acetonitrile and other organic solvents. The pretreatment processes of sample and the spectrum analyzing conditions are optimized. The samples are dehydrated by anhydrous sodium sulfate, then extracted by mixture solvents of acetone and n-hexane in 1 ： 1, filtered by organic membrane and tested by GC-MS. The result is that, in the concentration of 10~100 mg/L, the 6 insecticides all present good linear relationship and the correlation coefficient is 0.99. Through the recovery experiments of the water-borne varnish and water-borne woodenware coatings in the market, it is showed that the recovery rate of the method is 80.0%~99.6%, the relative standard deviation of the method is less than 5.0% and the detection limit is 0.38~1.96 mg/L. The method is simple, quick, sensitive and precise, and shows good effect.