中空纤维液相微萃取及血浆中文拉法辛及其代谢物的手性液相色谱-串联质谱分析
Hollow-fiber liquid-phase microextraction and chiral LC-MS/MS analysis of venlafaxine and its metabolites in plasma.
作者信息
da Fonseca Patrícia, Bonato Pierina Sueli
机构信息
Department of Physics & Chemistry, Faculty of Pharmaceutical Sciences of Ribeirão Preto, University of São Paulo, 14040-903, Ribeirão Preto, SP, Brazil.
出版信息
Bioanalysis. 2013 Mar;5(6):721-30. doi: 10.4155/bio.13.22.
BACKGROUND
An enantioselective analytical method was developed and validated for determination of venlafaxine and its metabolites O-desmethylvenlafaxine and N-desmethylvenlafaxine in plasma samples. The method employed LC-MS/MS analysis and hollow-fiber liquid-phase microextraction (HF LPME) for sample preparation.
RESULTS
After HF LPME optimization the following condition was established: sample volume of 4 ml, sample agitation at 1750 rpm, 20 min of extraction, 0.1 mol/l acetic acid as acceptor phase, 1-octanol as organic phase and donor phase pH adjustment to 10. Under these conditions, the method was linear over the concentration range of 5-500 ng/ml with quantification limits of 5 ng/ml.
CONCLUSION
The use of HF LPME for sample preparation provided suitable recoveries, efficient clean-up and low consumption of organic solvent.
背景
开发并验证了一种对映体选择性分析方法，用于测定血浆样品中的文拉法辛及其代谢物O-去甲基文拉法辛和N-去甲基文拉法辛。该方法采用液相色谱-串联质谱（LC-MS/MS）分析和中空纤维液相微萃取（HF LPME）进行样品制备。
结果
经过HF LPME优化后，确定了以下条件：样品体积4 ml，样品搅拌速度1750 rpm，萃取时间20分钟，0.1 mol/l乙酸作为接受相，1-辛醇作为有机相，供体相pH值调至10。在这些条件下，该方法在5-500 ng/ml浓度范围内呈线性，定量限为5 ng/ml。
结论
使用HF LPME进行样品制备具有合适的回收率、有效的净化效果和低有机溶剂消耗量。
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