血液中64种常见有机氯菊酯类农药的快速筛查

目的建立人体血浆中64种有机氯菊酯类农药多残留的气相色谱（GC）快速筛查分析方法。方法空白人体静脉抗凝血用乙腈沉淀蛋白,乙酸乙酯∶环己烷（v/v,3∶1）进行液液萃取净化,使用HP-5色谱柱,采用气相色谱进行定性、定量分析。对方法进行优化并进行方法学评价。结果 64种农药在0.001~0.1μg/mL范围内线性关系均良好,相关系数在0.990 1~0.999 9之间。检出限在0.001~0.15μg/mL范围内,方法定量限在0.001~0.5μg/mL之间,回收率总体于80%~110%之间,相对标准偏差小于15%,方法检出限总体于0.01μg/mL以下,日内精密度在1.5%~11.5%之间,日间精密度在2.9%~13.9%之间。结论本文建立的人体血浆的农药多残留快速筛查测定法,符合农药残留分析方法的要求,可在相关研究和实践中选用。

Rapid screening method of 64 organochlorine and pyrethroid pesticide residues analysis in human blood

Objective To establish a rapid screening method with gas chromatography （GC） to determine 64 organochlorine and pyrethroid pesticide residues in human plasma. Methods Liquid-liquid extraction was used with ethyl acetate： cyclohexane （v/v, 3：1 ） as solvent for extraction and purification. HP-5 capillary chromatography column was used for qualitative and quantitative analysis. Optimization the evaluation of the established methodology were approached. Results Linearity of 64 pesticides was observed over a range of 0. 001 - 0. 1 μg/mL with correlation coefficient between 0. 990 1 and 0. 999 9. Limits of detection ranged from 0. 001 and 0. 15 μg/mL and limits of quantification ranged from 0. 001 and 0.5 μg/mL. Recoveries overall ranged from 80% to 110%, and the relative standard deviation were all below 15%, the limits of detection were generally below 0. 01 μg/mL, the intra-day relative standard deviations ranged from 1.5% to 11.5%, and the inter-day relative standard deviations ranged from 2. 9% to 13.9%. Conclusion Rapid screening assay method for pesticide residues in human plasma established in this paper meet the requirements of pesticide residue analytical methods and can be used in relative research and practice.