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人血浆中尼卡地平的对映体选择性高效液相色谱测定法

Enantioselective high-performance liquid chromatographic determination of nicardipine in human plasma.

作者信息

Uno T, Ohkubo T, Sugawara K

机构信息

Department of Pharmacy, Hirosaki University Hospital, Japan.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 Sep 26;698(1-2):181-6. doi: 10.1016/s0378-4347(97)00277-6.

Abstract

A sensitive method for the enantioselective high-performance liquid chromatography (HPLC) determination of nicardipine in human plasma is described. (+)-Nicardipine, (-)-nicardipine and (+)-barnidipine as an internal standard are detected by an ultraviolet detector at 254 nm. Racemic nicardipine in human plasma was extracted by a rapid and simple procedure based on C18 bonded-phase extraction. The extraction samples were purified and concentrated on a pre-column using a C1 stationary phase and the enantiomers of nicardipine are quantitatively separated by HPLC on a Sumichiral OA-4500 column, containing a chemically modified Pirkle-type stationary phase. Determination of (+)- and (-)-nicardipine was possible in a concentration range of 5-100 ng ml(-1) and the limit of detection in plasma was 2.5 ng ml(-1). The recoveries of (+)- and (-)-nicardipine added to plasma were 91.4-98.4% and 93.3-96.7%, respectively, with coefficients of variation of less than 9.0 and 9.4% respectively. The method was applied to low level monitoring of (+)- and (-)-nicardipine in plasma from healthy volunteers.

摘要

描述了一种对映体选择性高效液相色谱(HPLC)法测定人血浆中尼卡地平的灵敏方法。(+)-尼卡地平、(-)-尼卡地平以及作为内标的(+)-巴尼地平通过紫外检测器在254 nm波长处进行检测。人血浆中的外消旋尼卡地平采用基于C18键合相萃取的快速简便方法进行萃取。萃取样品在预柱上使用C1固定相进行纯化和浓缩,尼卡地平对映体在含有化学修饰的Pirkle型固定相的Sumichiral OA - 4500柱上通过HPLC进行定量分离。(+)-和(-)-尼卡地平的测定浓度范围为5 - 100 ng/ml(-1),血浆中的检测限为2.5 ng/ml(-1)。添加到血浆中的(+)-和(-)-尼卡地平的回收率分别为91.4 - 98.4%和93.3 - 96.7%,变异系数分别小于9.0%和9.4%。该方法应用于健康志愿者血浆中(+)-和(-)-尼卡地平的低水平监测。

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