Simultaneous analyses of cocaine and its metabolite benzoylecgonine in urine by LC-MS/MS.
- Author:
Qi-ran SUN
1
;
Ping XIANG
;
Hui YAN
;
Min SHEN
Author Information
1. Department of Forensic Science, Shanghai Medical College, Fudan University, Shanghai 200032, China.
- Publication Type:Research Support, Non-U.S. Gov't
- MeSH:
Animals;
Chromatography, Liquid/methods*;
Cocaine/urine*;
Forensic Toxicology;
Guinea Pigs;
Humans;
Solid Phase Extraction;
Tandem Mass Spectrometry/methods*
- From:
Journal of Forensic Medicine
2008;24(4):268-272
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous analysis of cocaine (COC) and its metabolite benzoylecgonine(BZE) in urine samples.
METHODS:A single dose of COC (10 mg/kg) was injected intraperitoneally into guinea pigs and urine samples were collected for 7 days. The urine samples were extracted by auto solid phase extraction (SPE), separated by the Allure PFP propyl column with a mobile phase consisting of methanol and 20 mmol/L ammonium acetate buffer [0.1% formic acid (80:20, V/V)], and then analyzed by LC-MS/MS. Multiple reaction monitoring (MRM) mode was used to analyze COC (m/z 304.2-->182.3, m/z 304.2-->150.1) and BZE (m/z 290.2-->168.3, m/z 290.2-->105.0).
RESULTS:COC and BZE showed a fairly good linearity over the range of 2.0-100 ng/mL (r=0.9995). The detection limit was 0.5 ng/mL. The recovery rate was greater than 90% and the deviation of intra- and inter-day precision was less than 6%. BZE was the major target detected in urine samples, and its detection window was longer than COC.
CONCLUSION:This newly developed method shows high sensitivity and selectivity, and is suitable for the simultaneous analysis of cocaine and benzoylecgonine in urine samples.