顶空气相色谱法测定二氯乙酸二异丙胺尿药浓度

蔡素芳; 肖永红; 余泽波

doi:10.13406/j.cnki.cyxb.2004.01.035

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顶空气相色谱法测定二氯乙酸二异丙胺尿药浓度

更新时间：2024-01-17

- 顶空气相色谱法测定二氯乙酸二异丙胺尿药浓度
- Determination of diisopropylamide dichloroacetate concentrations in urine by GC-HS
- 重庆医科大学学报 2004年第1期页码：108-109
- 作者机构：
  
  1. 重庆医科大学临床学院感染科
  2. 重庆医科大学临床学院感染科,重庆,400016
- 作者简介：
- 基金信息：
- DOI：10.13406/j.cnki.cyxb.2004.01.035
  中图分类号： X830
- 纸质出版日期：2004，
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[1]蔡素芳,肖永红,余泽波.顶空气相色谱法测定二氯乙酸二异丙胺尿药浓度[J].重庆医科大学学报,2004(01):108-109+112.

CAI Sufang, et al. Determination of diisopropylamide dichloroacetate concentrations in urine by GC-HS[J]. Journal of Chongqing Medical University, 2004,(1):108-109.
[1]蔡素芳,肖永红,余泽波.顶空气相色谱法测定二氯乙酸二异丙胺尿药浓度[J].重庆医科大学学报,2004(01):108-109+112. DOI： 10.13406/j.cnki.cyxb.2004.01.035.

CAI Sufang, et al. Determination of diisopropylamide dichloroacetate concentrations in urine by GC-HS[J]. Journal of Chongqing Medical University, 2004,(1):108-109. DOI： 10.13406/j.cnki.cyxb.2004.01.035.

摘要

目的 :建立顶空气相色谱法测定尿中二氯乙酸二异丙胺浓度。方法 :AgilentDB - 5MS毛细管色谱柱（30m× 0 .2 5mm）

柱温 :4 0℃保持 2min

以 5℃ /min升至 80℃保持 2min

再以 2 0℃ /min升至 2 0 0℃保持 8min ;进样口温度 2 0 0℃

分流比 5∶1;氢火焰检测器

检测温度 30 0℃ ;载气为高纯N2

流速 1ml/min

H2 35ml/min

空气 35 0ml/min ;内标仲丁醇。结果 :标准曲线线性范围为 8～ 80 0 μg/ml

尿中二氯乙酸二异丙胺提取回收率为 88.75 %～ 98.0 6 %

相对回收率为 97.36 %～ 10 3.2 5 %

日内和日间RSD分别为 2 .95 %～ 6 .6 2 %和 2 .4 5 %～ 5 .6 1%

最低检测浓度为 2 μg/ml。结论 :该法操作简单

杂质干扰小

提取回收率高

适合于二氯乙酸二异丙胺尿药浓度的测定。

Abstract

Objective:To establish a method for determination of diisopropylamide dichloroacetate(DADA) concentrations in urine.Methods:GC-HS was applied to quantitative analysis.Using Agilent DB-5MS capillary column(30m×0.25mm)

the column temperature was ascended from 40℃ to 200℃ according to program.Initial temperature was 40℃ and maintained 2 mins

then temperature rose to 80℃ at 5℃/min rate and maintained 2 mins

finally temperature rose to 200℃ at 20℃/min rate and maintained 8 mins.The injector temperature was 200℃.The detector temperature was 300℃.Nitrogen was used as carrier gas

and the flow rate was 1 ml/min.The flow rate of hydrogen was 35 ml/min.The flow rate of air was 350 ml/min.An internal standard was secondary butanol.Results:The calibration curve was linear within 8～800μg/ml.The recovery rate of the extraction were 88.75%～98.06%.The recovery rate were 97.36%～103.25%。Within-day and between-day RSD were 2.95%～6.62% and 2.45%～5.61% respectively.Detectable concentration limited was 2μg/mL.Conclusion:The GC-HS method is simple

reliable

and suitable for urine DADA concentration analysis.

关键词

二氯乙酸二异丙胺尿药浓度顶空气相色谱法

Keywords

Diisopropylamide dichloroacetateDrug concentration in urineGC-HS

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