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Stacking and quantitative analysis of lovastatin in urine samples by the transient moving chemical reaction boundary method in capillary electrophoresis

机译:毛细管电泳中瞬态移动化学反应边界法对尿样中洛伐他汀的叠加和定量分析

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摘要

A simple, sensitive, and useful concentration method for lovastatin (Lvt) in urine has been developed based on the transient moving chemical reaction boundary method (tMCRBM) in capillary electrophoresis. The MCRB is formed with acidic sample buffer (Gly-HCl) and alkaline running buffer (Gly-NaOH). The following optimal conditions were determined for stacking and separation: electrophoretic buffer of 100 mM Gly- NaOH (pH 11.52), sample buffer of 20 mM Gly-HCl (pH 4.93), fused-silica capillary of 76 cm x 75-mu m i.d (67 cm from detector), sample injection at 14 mbar for 3 min. A 21- to 26-fold increase in peak height was achieved for detection of Lvt in urine under the optimal conditions compared with normal capillary zone electrophoresis. By combining the sample pretreatment procedure with the stacking method, the sensitivity of Lvt in urine was increased by 105- to 130-fold. The limits of detection (LOD) and quantification (LOQ) for Lvt in urine were decreased to 8.8 ng/mL and 29.2 ng/mL, respectively. The intra-day and inter-day precision values (expressed as RSD) were 2.23-3.61% and 4.03-5.05%, respectively. The recoveries of the analyte at three concentration levels changed from 82.65 to 100.49%.
机译:基于毛细管电泳中的瞬态移动化学反应边界法(tMCRBM),开发了一种简单,灵敏且有用的尿中洛伐他汀(Lvt)浓缩方法。 MCRB由酸性样品缓冲液(Gly-HCl)和碱性运行缓冲液(Gly-NaOH)组成。确定了以下最佳条件进行堆叠和分离:100 mM Gly-NaOH(pH 11.52)电泳缓冲液,20 mM Gly-HCl(pH 4.93)样品缓冲液,76 cm x75μmid的熔融石英毛细管(距检测器67厘米),在14毫巴下进样3分钟。与正常毛细管区带电泳相比,在最佳条件下检测尿液中Lvt的峰高增加了21至26倍。通过将样品预处理程序与堆积方法相结合,尿液中Lvt的灵敏度提高了105到130倍。尿液中Lvt的检出限(LOD)和定量限(LOQ)分别降至8.8 ng / mL和29.2 ng / mL。日内和日间精度值(表示为RSD)分别为2.23-3.61%和4.03-5.05%。三种浓度水平下分析物的回收率从82.65%变为100.49%。

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