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采用高效液相色谱-紫外检测法测定人血浆中西沙必利和去甲西沙必利的含量。

Determination of cisapride and norcisapride in human plasma using high-performance liquid chromatography with ultraviolet detection.

作者信息

Cisternino S, Schlatter J, Saulnier J L

机构信息

Department of Pharmacy, Hospital of Gonesse, France.

出版信息

J Chromatogr B Biomed Sci Appl. 1998 Sep 4;714(2):395-8. doi: 10.1016/s0378-4347(98)00213-8.

DOI:10.1016/s0378-4347(98)00213-8
PMID:9766883
Abstract

A simple, rapid and reproducible high-performance liquid chromatographic assay for cisapride and norcisapride in human plasma is described. Samples of plasma (150 microl) were extracted using a C18 solid-phase cartridge. Regenerated tubes were eluted with 1.0 ml of methanol, dried, redissolved in 150 microl of methanol and injected. Chromatography was performed at room temperature by pumping acetonitrile-methanol-0.015 M phosphate buffer pH 2.2-2.3 (680:194:126, v/v/v) at 0.8 ml/min through a C18 reversed-phase column. Cisapride, norcisapride and internal standard were detected by absorbance at 276 nm and were eluted at 4.3, 5.3 and 8.1 min, respectively. Calibration plots in plasma were linear (r>0.998) from 10 to 150 ng/ml. Intraday precisions for cisapride and norcisapride were 3.3% and 5.4%, respectively. Interday precisions for cisapride and norcisapride were 9.6% and 9.0%, respectively. Drugs used which might be coadministered were tested for interference.

摘要

本文描述了一种用于测定人血浆中西沙必利和去甲西沙必利的简单、快速且可重复的高效液相色谱法。取150微升血浆样本,用C18固相柱进行萃取。用1.0毫升甲醇洗脱再生柱,吹干,再用150微升甲醇重新溶解并进样。在室温下进行色谱分析,以0.8毫升/分钟的流速将乙腈-甲醇-0.015M pH 2.2 - 2.3的磷酸盐缓冲液(680:194:126,v/v/v)泵入C18反相柱。通过在276纳米处的吸光度检测西沙必利、去甲西沙必利和内标物,它们的洗脱时间分别为4.3分钟、5.3分钟和8.1分钟。血浆中的校准曲线在10至150纳克/毫升范围内呈线性(r>0.998)。西沙必利和去甲西沙必利的日内精密度分别为3.3%和5.4%。西沙必利和去甲西沙必利的日间精密度分别为9.6%和9.0%。对可能同时给药的所用药物进行了干扰测试。

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