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阳离子交换色谱后溶剂萃取-气相色谱-质谱联用测定有机酸

GC-MS determination of organic acids with solvent extraction after cation-exchange chromatography.

作者信息

Suh J W, Lee S H, Chung B C

机构信息

Doping Control Center, Korea Institute of Science and Technology, Cheongryang, Seoul, Korea.

出版信息

Clin Chem. 1997 Dec;43(12):2256-61.

PMID:9439441
Abstract

We combined column and partition chromatography to isolate, purify, and quantify biological organic acids in urine and cerebrospinal fluid (CSF). Urine and CSF samples were introduced onto a preconditioned cation-exchange column (Dowex 50 W x 8 resin) to remove the biological interferences. The effluent with water was extracted with ethyl acetate two times (pH 1 and 3) and the organic acids were quantitatively converted into their trimethylsilyl derivatives for detection by gas chromatography-mass spectrometry. The good quality-control data were obtained through precision and accuracy tests. Inter- and intraassay CVs were 0.01-10.2% and 0.02-12.2%, respectively. Analytical recoveries compared favorably with results from the commonly used solvent extraction method. This method was used for the measurement of the 14 organic acids in the urine and CSF of healthy volunteers. The values obtained were in the range of the published data.

摘要

我们结合柱色谱法和分配色谱法来分离、纯化和定量尿液和脑脊液(CSF)中的生物有机酸。将尿液和脑脊液样本引入预处理过的阳离子交换柱(Dowex 50 W x 8树脂)以去除生物干扰物。用水冲洗后的流出物用乙酸乙酯萃取两次(pH值为1和3),并且将有机酸定量转化为其三甲硅烷基衍生物,用于通过气相色谱 - 质谱法进行检测。通过精密度和准确度测试获得了良好的质量控制数据。批间和批内变异系数分别为0.01 - 10.2%和0.02 - 12.2%。分析回收率与常用溶剂萃取法的结果相比具有优势。该方法用于测量健康志愿者尿液和脑脊液中的14种有机酸。获得的值在已发表数据的范围内。

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GC-MS determination of organic acids with solvent extraction after cation-exchange chromatography.阳离子交换色谱后溶剂萃取-气相色谱-质谱联用测定有机酸
Clin Chem. 1997 Dec;43(12):2256-61.
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[Study of the extraction of organic acids from urine. Preliminary step to their gas chromatographic separation (author's transl)].[尿液中有机酸的提取研究。气相色谱分离的初步步骤(作者译)]
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