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采用固相萃取-高效液相色谱法测定人血浆中戊烯醇含量。

Determination of ng rivanol in human plasma by SPE-HPLC method.

作者信息

Guo Zhiyong, Wei Danyi, Gan Ning, Xie Hongzhen, Yu Xufei

机构信息

Faculty of Materials Science and Chemical Engineering, The State Key Laboratory Base of Novel Functional Materials and Preparation Science, Ningbo University, 315211 Ningbo, China.

出版信息

J Chromatogr Sci. 2007 Jul;45(6):325-9. doi: 10.1093/chromsci/45.6.325.

Abstract

A high-performance liquid chromatography assay is described for the determination of rivanol in human plasma. Solid-phase extraction cartridges are used to extract plasma samples. Separation is done by using a C18 column. The mobile phase is a mixture of methanol-0.05% sodium dodecylsulfonate (70:30, v/v, pH 3), with the flow rate at 1.0 mL/min. UV detection of rivanol is at 272 nm. The calibration curve is linear in the concentration range of 1x10(-8) mol/L to 1x10(-5) mol/L with linear correlation coefficient r equal to 0.9998. The limit of detection for the assay is 3x10(-9) mol/L, corresponding to 1.1 ng/mL. Precision, expressed as the within- and between-day coefficient of variation, is 3.3-8.1% and 4.1-9.5%, respectively, at plasma control samples of 5x10(-8), 5x10(-7), and 5x10(-6) mol/L. And the recovery ranges from 94.8% to 107.2%. The selectivity of the method is confirmed. Plasma samples are stable for at least 15 days if they are stored lightproof at -20 degrees C. This method is simple, sensitive, and accurate, and it allows for the determination ng rivanol in human plasma. It could be applied to assessing its plasma level in women receiving an intra-amniotic injection of rivanol.

摘要

本文描述了一种用于测定人血浆中利凡诺的高效液相色谱法。采用固相萃取柱提取血浆样品。使用C18柱进行分离。流动相为甲醇 - 0.05%十二烷基磺酸钠(70:30,v/v,pH 3)的混合物,流速为1.0 mL/min。利凡诺的紫外检测波长为272 nm。校准曲线在1x10(-8) mol/L至1x10(-5) mol/L的浓度范围内呈线性,线性相关系数r等于0.9998。该测定方法的检测限为3x10(-9) mol/L,相当于1.1 ng/mL。在5x10(-8)、5x10(-7)和5x10(-6) mol/L的血浆对照样品中,日内和日间变异系数分别表示的精密度为3.3 - 8.1%和4.1 - 9.5%。回收率在94.8%至107.2%之间。该方法的选择性得到了证实。血浆样品在-20℃避光保存至少15天是稳定的。该方法简单、灵敏、准确,可用于测定人血浆中纳克级的利凡诺。它可应用于评估接受羊膜腔内注射利凡诺的女性的血浆水平。

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