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固相萃取后测定人血浆中维拉帕米的高效液相色谱法。

HPLC method for determination of verapamil in human plasma after solid-phase extraction.

作者信息

Ivanova Violeta, Zendelovska Dragica, Stefova Marina, Stafilov Trajce

机构信息

Institute of Chemistry, Faculty of Science, Sts. Cyril and Methodius University, POB 162, 1000 Skopje, Republic of Macedonia.

出版信息

J Biochem Biophys Methods. 2008 Apr 24;70(6):1297-303. doi: 10.1016/j.jbbm.2007.09.009. Epub 2007 Oct 6.

Abstract

A simple, rapid and precise HPLC method has been developed for the assay of verapamil in human plasma. The clean up of the plasma samples was tested using several adsorbents for solid-phase extraction and best recovery was obtained using mixed-mode cartridges (HLB - hydrophilic-lipophilic balance) ranging between 94.70 and 103.71%. HPLC separation was performed with isocratic elution on Lichrospher 60 RP-select B column (250 mm x 4 mm I.D., 5 microm particle size). The mobile phase was 40% acetonitrile and 0.025 mol/L KH2PO4 with pH 2.5 at flow rate of 1 mL/min. Diltiazem was used as internal standard and the detection wavelength was 200 nm. The calibration curves were linear in the range of 10-500 ng/mL. The developed method is convenient for routine analysis of verapamil in human plasma.

摘要

已开发出一种简单、快速且精确的高效液相色谱(HPLC)方法用于测定人血浆中的维拉帕米。使用多种吸附剂进行固相萃取以测试血浆样品的净化效果,使用混合模式柱(HLB - 亲水亲脂平衡)获得了最佳回收率,回收率在94.70%至103.71%之间。在Lichrospher 60 RP-select B柱(250 mm×4 mm内径,5微米粒径)上采用等度洗脱进行HPLC分离。流动相为40%乙腈和0.025 mol/L磷酸二氢钾,pH 2.5,流速为1 mL/min。地尔硫卓用作内标,检测波长为200 nm。校准曲线在10 - 500 ng/mL范围内呈线性。所开发的方法便于对人血浆中的维拉帕米进行常规分析。

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