科研之友
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摘要
Presently urine analysis for methadone and its metabolite 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) is performed for emergency toxicology screening and pain management compliance testing (PMCT). Presented is the validation of a high-pressure liquid chromatography with tandem mass spectrometry method for methadone and EDDP in urine. Samples were simply diluted 1:1 (v:v) with 0.1 mu g/mL of methadone-d(3) and EDDP-d(3) in methanol before analysis. The chromatographic separation was performed using a Pinnacle C18 100x3.2mm, 3 mu m column with a mobile phase containing water/acetonitrile (20:80v:v) with 1% formic acid delivered at a flow rate of 0.5mL/min. Detection was accomplished by multiple-reaction monitoring via electrospray ionization source operating in the positive ionization mode. The calibration curve was linear over the investigated concentration range, 25 to 5000ng/mL, for both methadone and EDDP. The lower limit of quantitation for each analyte was 25ng/mL. The intra- and inter-day precisions had coefficient of variations less than 15% and the accuracy was within the range from 94% to 110%. The method proved adequate for methadone and EDDP analysis of urine for emergency clinical toxicology and PMCT.
- 出版日期2014-4-21
