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固相萃取-衍生化-气相色谱法测定血液中的3种苯氧羧酸类除草剂 被引量:14

Determination of three phenoxyalkanoic acid herbicides in blood using gas chromatography coupled with solid-phase extraction and derivatization
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摘要 建立了一种血液中2,4-二氯苯氧乙酸(2,4-D)、2-(2,4-二氯苯氧)-丙酸(2,4-DP)和4-氯-2-甲基-苯氧乙酸(MCPA)3种苯氧羧酸类除草剂的分析方法。血样用0.1mol/L盐酸稀释后用GDX401大孔树脂吸附、用乙醚洗脱,萃取物用二氯丙醇在硫酸催化下进行酯化衍生,衍生物经气相色谱-电子捕获检测。2,4-D、2,4-DP和MCPA的检测限分别为20,8和40ng/mL。定量分析用2,4-二氯苯乙酸作内标,线性关系和回收率结果均令人满意。 A method for the determination of three phenoxyalkanoic acid herbicides, 2,4-dichlorophenoxyacetic acid ( 2,4-D), 2- (2,4-dichlorophenoxy) -propanoic acid ( 2,4-DP), and 4- chloro-2-methylphenoxy-acetic acid (MCPA) , in blood was developed. The blood sample was diluted with 0.1 mol/L hydrochloric acid, and extracted by solid-phase extraction using porous resin GDX401 as adsorbent and ethyl ether as eluent. The extract was esterified with dichloropropanol in the presence of sulfuric acid as catalyst. The derivatives were analysed by gas chromatography with electron-capture detection. The detection limits of 2,4-D, 2,4-DP and MCPA were 20, 8 and 40 ng/mL, respectively. In quantitative analysis, 2,4-dichlorophenylacetic acid was used as an internal standard. The linear relationships and recoveries were satisfactory. The derivatization of the three herbicides with methanol, ethanol, n-propanol, n-butanol, and trif- luoroethanol were also studied, and the analytical methods of these derivatization were compared with that of dichloropropanol as esterifying agent. The method is sensitive enough for the examination of the poison samples in actual.
出处 《色谱》 CAS CSCD 北大核心 2008年第1期116-118,共3页 Chinese Journal of Chromatography
基金 公安部科研课题(No.20029323101)
关键词 固相萃取 酯化衍生化 气相色谱法 苯氧羧酸类除草剂 血液 solid-phase extraction (SPE) esterifying derivatization gas chromatography ( GC ) phenoxyalkanoic acid herbicides blood
作者简介 辛国斌,硕士研究生. 通讯联系人:谭家镒,教授.E-mail:ccpctjy@yahoo.com.cn.
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