血清中2,4-滴丁酯测定的气相色谱法

Method for determining 2, 4-D butylate in serum by gas chromatography

目的 建立血清中2,4-滴丁酯测定的气相色谱法,为临床中毒的诊断和救治提供依据.方法 取0.5 ml血清加三氯甲烷2.0 ml充分振荡萃取,静置5 min,4 000 r/min离心10 min,取三氯甲烷层氮气吹干.50μl乙醇定容,1.0μl进样,氢火焰检测器气相色谱法测定.结果 血清中2,4-滴丁酯浓度在5～40 μg/ml范围内呈线性,回归方程y=1831.6.4x-899.4,r=0.9992,最低检出浓度1.0 μg/ml.方法回收率为88.7％～103.0％；相对标准偏差（RSD）为3.8％～5.0％.日内、日间RSD分别为3.87％～4.92％和3.33％～5.34％.结论 该方法操作简便、分析快速,结果准确.为快速诊断和治疗2,4-滴丁酯中毒提供了很好的检测方法.

Objective To establish a method for determining 2,4-D butylate in serum by gas chromatography （GC） and to provide a basis for the diagnosis and treatment of clinical poisoning.Methods Serum 2,4-D butylate level was determined by the following steps：mixing serum （0.5 ml） with trichloromethane （2.0 ml）,adequately shaking for extraction,standing for 5 min,centrifuging at 4 000 rpm for 10 min,blowdrying the trichloromethane layer with nitrogen,adding ethanol （50 μl） to a certain volume,adding the sample （1.0 μl）,and performing GC with a hydrogen flame ionization detector.Results Serum 2,4-D butylate level showed a linear relationship within 5～40 μg/ml,with a regression equation of y=1 831.6.4x-899.4 （r=0.999 2）; the minimum detectable concentration was 1.0 μg/ml.The recovery rate was 88.7％～103.0％ （relative standard deviation （RSD） 3.8％～5.0％）.The intra-day RSD and inter-day RSD were 3.87-4.92％ and 3.33％～5.34％,respectively.Conclusion This determination method is simple,efficient,and accurate and provides a good means for rapid diagnosis and treatment of 2,4-D butylate poisoning.