Performance of a pentafluorophenylpropyl stationary phase for the electrospray ionization high-performance liquid chromatography-mass spectrometry-mass spectrometry assay of cocaine and its metabolite ecgonine methyl ester in human urine

被引:41
作者
Needham, SR
Jeanville, PM
Brown, PR
Estape, ES
机构
[1] Pfizer Inc, Div Cent Res, Drug Metab Technol Grp, Groton, CT 06340 USA
[2] Univ Rhode Isl, Dept Chem, Kingston, RI 02881 USA
[3] Univ Puerto Rico, Coll Hlth Related Profess, San Juan, PR 00936 USA
来源
JOURNAL OF CHROMATOGRAPHY B | 2000年 / 748卷 / 01期
关键词
stationary phases; LC; cocaine; ecgonine methyl ester; pentafluorophenylpropyl;
D O I
10.1016/S0378-4347(00)00271-1
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A pentafluorophenylpropyl (PFPP) bonded silica column has been used for the high-performance liquid chromatography-electrospray ionization-mass spectrometry-mass spectrometry assay (HPLC-ESI-MS-MS) of cocaine (COC) and its metabolite, ecgonine methyl ester (EME) in human urine. COC and EME were used as model basic solutes to demonstrate that a PFPP phase yields excellent results for the assay and validation of drugs in biological fluids, The assay was linear over three orders of magnitude (1.0-1000 ng/ml) and precision and accuracy of the assay was 4 and 15%, respectively. The limit of detection (LOD) for COC and EME was 1.6 and 2.8 pg on column, respectively. In addition, only a simple 1:10 dilution of the urine was necessary for the sample preparation procedure thus saving time on a laborious extraction step. The major advantage of the PFPP phase was the enhancement of the ESI-MS signal by providing good retention and good peak shape of COC and EME with a mobile phase of 90% acetonitrile. The MS signal for COC was a factor of 12 times greater on the PFPP phase than on the C-18 phase. (C) 2000 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:77 / 87
页数:11
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