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尿液中氯噻酮的在线固相萃取-高效液相色谱测定法

On-line solid-phase extraction and high-performance liquid chromatographic determination of chlorthalidone in urine.

作者信息

Salado S, Vera-Avila L E

机构信息

Centro A.F. de Estudios Tecnológicos S.A., Mexico D.F., Mexico.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):195-202. doi: 10.1016/s0378-4347(96)00396-9.

DOI:10.1016/s0378-4347(96)00396-9
PMID:9106044
Abstract

A simple and rapid on-line method for the determination of chlorthalidone in urine is proposed. The sample containing the internal standard is injected in a CN precolumn. After a 2-ml water rinsing, the precolumn is coupled for 30 s to the HPLC column via a switching, valve, allowing the on-line elution of the compounds of interest. Analysis is carried out by reversed-phase chromatography with an acetonitrile-0.01 M phosphate buffer pH 7 (20:80, v/v) eluent, using UV detection at 214 nm. While the LC separation is performed, the precolumn is regenerated and conditioned, and is ready to receive the next sample at the end of the run. Accurate (> 95%) and precise (< 10%) analyses, in the range of 0.1-20 micrograms/ml of chlorthalidone in urine, have been achieved using this method.

摘要

提出了一种简单快速的尿液中氯噻酮在线测定方法。将含有内标的样品注入氰基预柱。用2毫升水冲洗后,通过切换阀将预柱与高效液相色谱柱连接30秒,使感兴趣的化合物在线洗脱。采用反相色谱法,以乙腈-0.01M pH 7磷酸盐缓冲液(20:80,v/v)为洗脱剂,在214nm处进行紫外检测。在进行液相色谱分离时,预柱进行再生和调节,运行结束时即可接收下一个样品。使用该方法在尿液中氯噻酮浓度为0.1-20微克/毫升的范围内实现了准确(>95%)和精密(<10%)的分析。

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