Automated solid-phase extraction method for the determination of piperaquine in plasma by peak compression liquid chromatography
Automated solid-phase extraction method for the determination of piperaquine in plasma by peak compression liquid chromatography
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DOI：
10.1093/chromsci/41.1.44
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发表时间：
2003-01-01
影响因子：
1.3
通讯作者：
Bergqvist, Y
中科院分区：
文献类型：
--
作者：
Lindegårdh, N;Ashton, M;Bergqvist, Y
建立了固相萃取-液相色谱峰压缩法测定血浆中哌喹（PQ）的生物分析方法。用乙腈-1%醋酸水溶液（85：15，v/v）从血浆中沉淀蛋白质。在将样品上样到强阳离子交换剂（Isolute PRS）SPE色谱柱之前，向样品中加入内标物（IS）。在Zorbax SB-CN色谱柱（250 × 4.0 mm）上，采用移动的流动相乙腈-磷酸盐缓冲液[I = 0.1，pH 2.5（12：88，v/v）]和UV检测器（345 nm），通过LC分析PQ和IS。在进样至色谱系统之前，向样品中加入三氯乙酸（TCA）。PQ以TCA的梯度洗脱，这使得能够压缩PQ的峰值，从而显著提高峰值效率。血浆的测定内精密度在3.00µM和0.050µM下分别为5.4%和5.8%。血浆的批间精密度在3.00µM和0.050µM下分别为1.3%和10.0%。定量下限和检测限分别为0.025和0.005µM。
A validated bioanalytical method for the determination of piperaquine (PQ) in plasma by solid-phase extraction (SPE) and liquid chromatography (LC) using peak compression is presented. Protein is precipitated from plasma with acetonitrile-1% aqueous acetic acid (85:15, v/v). An internal standard (IS) is added to the samples before they are loaded onto a strong cation exchanger (Isolute PRS) SPE column. PQ and the IS are analyzed by LC on a Zorbax SB-CN column (250 × 4.0 mm) with the mobile phase acetonitrile.phosphate buffer [I = 0.1, pH 2.5 (12:88, v/v)] and UV detection at 345 nm. Trichloroacetic acid (TCA) is added to the samples prior to injection into the chromatography system. PQ elutes in a gradient of TCA, which enables peak compression of PQ and significantly higher peak efficiency as a result. The intraassay precision for plasma is determined to be 5.4% at 3.00µM and 5.8% at 0.050µM. The interassay precision for plasma is 1.3% at 3.00µM and 10.0% at 0.050µM. The lower limit of quantitation and the limit of detection are 0.025 and 0.005µM, respectively.