Chinese Journal of Chromatography

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Simultaneous determination of stimulant, narcotics and antiestrogen in urine by gas chromatography-nitrogen phosphorous detection

QIU Lijun1, ZHENG Xiaoyan2, YOU Feiming2, LIU Wei1, ZHANG Jinzhang1, ZHANG Lan1*   

  1. 1.Key Laboratory of Analysis and Detection for Food Safety, Fuzhou University, Fuzhou 350002, China; 2.Fujian Provincial Central Inspection Institute, Fuzhou 350002, China
  • Received:2008-10-08 Revised:2008-12-08 Online:2009-05-30 Published:1982-09-25
  • Contact: ZHANG Lan

Abstract: An easy, sensitive and quick method was established for simultaneously separating and determining stimulant, narcotics and antiestrogen in spiked human urine using gas chromatography-nitrogen phosphorous detection (GC-NPD). The urine sample was preprocessed by liquid-liquid extraction. Tert-butyl methyl ether and N-phenylamine were chosen as extraction solvent and internal standard for quantitation, respectively. That is, a standard stock mixture containing methylephedrine, meperidine, methadone, tamoxifen, fentanyl and N-phenylaniline was added into 5.0 mL urine samples and mixed uniformly, then 0.5 mL 5.0 mol/L NaOH, 3.0 g NaCl and 5.0 mL tert-butyl methyl ether were added and finally centrifuged. The extraction solution was dried under N2, redissolved by acetone and then determined by GC-NPD. The method showed the satisfactory linearity was between 0.022~20 mg/L, with the coefficient correlation from 0.9945 to 0.9998. The detection limits were in the range of 0.007~0.015 mg/L, and the average recoveries in spiked urine were between 75.8%~118.2% and the relative standard deviations were lower than 17.2%.

Key words: antiestrogen, doping, narcotics, stimulant, urine , gas chromatography-nitrogen phosphorous detection