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目的建立采用漩涡辅助液液微萃取前处理技术,GC-ECD为色谱检测仪器,测定环境水样中有机氯和菊酯类农药残留的分析方法。方法方法考察了萃取剂种类、萃取体积、萃取时间、漩涡速度、盐浓度对萃取效率的影响,对各种影响条件进行了优化,确定了最佳萃取条件为:在25 ml容量瓶中依次加入1 g NaCl,20 ml水样,再用微量注射器加100μl萃取剂正己烷,在2500 r/min旋涡2 min,静置分层,萃取层供色谱分析。结果该方法在0.05 mg/L~1.00 mg/L浓度范围内呈良好的线性关系,线性相关系数为0.995~0.999,方法检出限为0.005μg/L~0.1μg/L(S/N=3),方法的添加回收率为85%~110%,6次平行测定的相对标准偏差为3.5%~10%。结论操作简单、快速、成本低、环保高效、富集效率高等优点,能满足环境水样中有机氯和菊酯类农药检测需要。
OBJECTIVE To establish a method for the determination of organochlorine and pyrethroid pesticide residues in environmental water samples by using swirl-assisted liquid-liquid microextraction and preconditioning techniques and GC-ECD as chromatographic instrumentation. Methods The effects of extractant type, extraction volume, extraction time, vortex velocity and salt concentration on extraction efficiency were investigated. Various influence conditions were optimized. The optimal extraction conditions were as follows: 25 ml volumetric flask 1 g of NaCl, 20 ml of water sample, and then using a micro syringe with 100 μl of n-hexane, vortexed at 2500 r / min for 2 min, allowed to stand for delamination and extraction for chromatographic analysis. Results The method showed a good linearity in the range of 0.05 mg / L ~ 1.00 mg / L with a linear correlation coefficient of 0.995 ~ 0.999. The detection limit was 0.005 μg / L ~ 0.1 μg / L (S / N = 3 ), The recoveries of the method were 85% ~ 110%, and the relative standard deviations of six parallel determinations were 3.5% ~ 10%. Conclusions Simple, fast, low cost, high environmental efficiency and high enrichment efficiency can meet the need of detecting organochlorine and pyrethroid pesticides in environmental water samples.