期刊
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
卷 878, 期 28, 页码 2811-2816出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2010.08.032
关键词
Hollow fiber liquid-phase microextraction; High-performance liquid chromatography; Aconitine; Hypaconitine; Mesaconitine; Urine sample
资金
- National Nature Science Foundation of China [20875095]
- National Key Technology Research and Development Program of China [2007BA137B05]
- Chinese Academy of Sciences
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.
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