Determination of aconitine, hypaconitine and mesaconitine in urine using hollow fiber liquid-phase microextraction combined with high-performance liquid chromatography
Determination of aconitine, hypaconitine and mesaconitine in urine using hollow fiber liquid-phase microextraction combined with high-performance liquid chromatography
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中空纤维液相微萃取-高效液相色谱法测定尿液中乌头碱、次乌头碱和新乌头碱
DOI：
10.1016/j.jchromb.2010.08.032
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发表时间：
2010-10-15
影响因子：
3
通讯作者：
Shi, Yan-Ping
中科院分区：
文献类型：
--
作者：
Yang, Yang;Chen, Juan;Shi, Yan-Ping
建立了中空纤维液相微萃取(HF-LPME)-高效液相色谱法同时测定尿样中乌头碱(AC)、次乌头碱(HA)和中乌头碱(MA)的方法。从含1.0mmo1/L氢氧化钠的5mL尿样中提取分析物到浸渍在中空纤维壁孔内的正辛醇膜相中，然后反萃取到中空纤维管腔内的酸化水溶液中。提取后，用高效液相色谱法直接测定10亩L的受体相。在该方法中，对有机溶剂、萃取时间、搅拌速度、供体相和受体相的pH值、温度和受体相的体积等重要的萃取参数进行了优化。该方法在提取60min内浓缩倍数为98~288倍，重复性好，RSD为0.99~7.22%。人尿中AC、HA和MA的线性范围分别为16.0~128.0、11.0~88.0mg/L和8.1~64.8mg/L，相关系数分别为0.9949、0.9969和0.9904。尿样加标回收率AC为84.4%~106.2%，HA为77.3%~85.6%，MA为90.1%~100.8%。(C)2010爱思唯尔B.V.保留所有权利。
Hollow fiber liquid-phase microextraction (HF-LPME) coupled with high-performance liquid chromatography was used to simultaneously determine three Aconitum alkaloids, including aconitine (AC), hypaconitine (HA) and mesaconitine (MA) in human urine sample. Analytes were extracted from 5 mL urine sample containing 1.0 mmol/L NaOH into 1-octanol membrane phase impregnated in the pores of hollow fiber wall, and then back extracted into acidified aqueous solution in the lumen of the hollow fiber. After extraction, 10 mu L of the acceptor phase was analyzed directly by HPLC. In this method, some important extraction parameters,such as organic solvent, extraction time, stirring rate, pH of donor phase and acceptor phase, temperature, and the volume of acceptor phase were optimized. This method provided 98- to 288-fold enrichment factors within 60 min of extraction and good repeatability with RSDs of 0.99-7.22%. The calibration curves were linear over the ranges of 16.0-128.0 mu g/L for AC, 11.0-88.0 mu g/L for HA and 8.1-64.8 mu g/L for MA in human urine sample, with correlation coefficients of 0.9949, 0.9969 and 0.9904, respectively. Limits of detection were from 0.7 to 1.5 mu g/L, and recoveries from spiked urine sample varied from 84.4% to 106.2% for AC, 77.3% to 85.6% for HA and 90.1% to 100.8% for MA. (C) 2010 Elsevier B.V. All rights reserved.