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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。
Objective To establish a gas chromatography (GC) rapid screening assay for 64 residues of permethrin pesticides in human plasma. Methods Blank human venous anticoagulants were purified by liquid-liquid extraction with acetonitrile-precipitated protein and ethyl acetate: cyclohexane (v / v, 3: 1). Qualitative and quantitative analysis was performed by gas chromatography with HP-5 column. Method optimization and methodological evaluation. Results The linear relationships of 64 kinds of pesticides in the range of 0.001-0.1 μg / mL were good with the correlation coefficients between 0.990 1 and 0.999 9. The limits of detection were in the range of 0.001-0.15 μg / mL. The limits of quantification were in the range of 0.001-0.5 μg / mL. The recoveries were in the range of 80% -110%. The relative standard deviations were less than 15% At 0.01μg / mL, the intra-day precision was between 1.5% and 11.5%, and the intra-day precision was between 2.9% and 13.9%. Conclusion The rapid determination of pesticide residues in human plasma established in this paper is in line with the requirements of pesticide residue analysis methods and can be used in related research and practice.