血清中敌敌畏检测的气相色谱法

Method for determining concentration of dichlorvos in serum by gas chromatography

目的建立血清中敌敌畏浓度检测的气相色谱法，为临床诊断和监测提供定量依据。方法取0．5ml血清加乙酸乙酯2．0ml充分震荡萃取，静置5min，4000r／min离心，取上清液，氮气吹干，50μl乙醇定容，取1．0μl进样玻璃填充柱，用氮磷检测器检测和气相色谱法分析。结果血清中敌敌畏浓度在5．0．50．0μg／ml范围内呈线性关系，回归方程y=804．13x-691．8，r=0.9992。最低检出浓度为2．0μg／ml，回收率为86．8％～94．5％，相对标准偏差（RSD）为4．6％～5．5％。日内、日间RSD分别为4．52％～5．21％和3．56％～5．52％。结论该方法操作简便、分析快速，结果准确，适于临床的快速诊断敌敌畏中毒和量化评估治疗效果。

Objective To develop a method for determining the concentration of dichlorvos in serum by gas chromatography and to provide a basis for clinical diagnosis and monitoring of dichlorvos poisoning.Methods The serum （0.5 ml） collected from patients with dichlorvos poisoning was mixed with ethyl acetate （2.0 ml） and underwent shaking/extraction; the obtained liquid was subjected to standing （5 min） and centrifuging （4000 rpm）; the obtained supernatant was collected and blow-dried with nitrogen and was then dissolved in ethanol （50 μl）; 1.0 μl of the obtained liquid was collected and loaded into a glass-packed column; gas chromatography was performed using a nitrogen-phosphorus detector. Results A linear relationship was found when the concentration of dichlorvos in serum was 5.0-50.0 μg/ml, with a regression equation of y= 804.13x-691.8 （r=-0.9992）. The minimum detectable concentration was 2.0 μg/ml, the recovery rate was 86.8%-94.5%, the relative standard deviation （RSD） was 4.6%-5.5%, with an intra-day RSD of 4.52%-5.21% and an inter-day RSD of 3.56%-5.52%. Conclusion This determination method is easy to operate, efficient, and accurate, and can be used for quickly diagnosing dichlorvos poisoning and quantitatively evaluating treatment oil｜come.