Qualitative Examination Of Amfetamine And Ephedrine In Urine In Doping Using Gas Chromatography-Mass Spectrometry Method
Keywords:
Amphetamines, ephedrine, gas chromatography-mass spectrometryAbstract
Amphetamines and ephedrine are stimulant class doping drugs which have the effect of reducing fatigue and drowsiness, increasing alertness, physical strength, mental sense of competition and competitive attitude. Analysis of doping drugs in urine that has been recommended by the International Olympic Committee, including Gas Chromatography-Mass Spectrometry. Derivatization is carried out to change the polarity of the analyte, making it easier to become a gas and stable to heating. This study was conducted for qualitative analysis of amphetamine and ephedrine, using an HP5MS column containing non-polar phenyl methyl siloxane, temperature 100-250oC with a temperature increase of 10oC/minute. Then it was extracted with a mixture of diethyl ether-ethylacetate (1:1) in an alkaline medium pH 8, the organic layer was evaporated then derivatized with trifluoro-acetic acid-anhydride and ephedrine with acetic-anhydride-pyridine (3:2). The final results showed that the retention times of amphetamine and ephedrine were 10.47 and 4.9 minutes. While the derivatives are 13.34 and 5.50 minutes. Identification using mass spectrometry for each compound showed that the mass spectra matched the Ref. and the amphetamine and ephedrine structural similarity index was 96% and the detection limit for each compound was 2 ug/ml.
References
April SY Wong, et all., Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry., Drug Test Anal. 2017,(9) : 1320-1327.
Aronson, JK, 2014, Side Effects of Drugs Annual 35, University of Oxford, Elsivier.
Bellotti, B, Benzi,G., and Jungopist,L., World Symposium on Doping in Sport International Athletic Foundation, Montle Carlo, 5-7 June 1989, Official Proceedings of International Federation (IAF), 1990 :1-193.
Donike, M., and Stratmann, D., Identification of Stimulant Drugs with Phenoalkylamine Structure by Retention Indices, J. Anal. Chem., 279(2),1976,50-56.
Gandjar, IB and Rohman, A. 2010. Pharmaceutical Chemistry Analysis. Yogyakarta: Student Library.
Handajani, MS2006., Amphetamines and their derivatives. Jakarta
Harris, N., and Lovesey, J., The Sports Health Handbook, World Work Ltd., London, 1982, 17-19, 57-60.
Hong, J., Seok, DL, Kee, PH, Jeong, AL, and Jongsei, P., Determination of Phenoalkyamines, Narcotic Analgesics and Beta Blokers by Gas Chromatography-Mass Spectrometry, J.Anal.Toxicol., 14(3) , 1990, 77-83.
IDAADCandraningrat, et al; Review of the Ability of the GC-MS Method in the Identification of Flunitrazepam Related to Forensic and Clinical Aspects; Journal of Chemistry; 15(1), January, 2021 : 12-17.
Lucia Politi, et all: Application of Liquid Chromatography-Mass Spectrometry in Doping Control, Journal of Anal.Tox,Vol.29,January,2005 : 1-14.
Made Agus Gelgel Wirasuta: Forensic Toxicological Analysis and Interpretation of Analysis Findings; Indonesian Journal of Legal and forensic Science,I (1) 2008 : 47-55.
Chromatographic Method, Dwiarso Rud Yanto, Deeppublish, 2017.
Park,J., Sonja., and Lho, DS, Drug Testing at the 10th Asian Games and 24th Seoul Olympic Games, J. Anal. Toxicol., 14(3), 1990, 66-72.
Saito,T., Morita,T., Inoue,S., Yamamoto,I., and Inokuchi, S., 2008 : GC-MS assay for acetaminophen in human hair segment, Forensix Toxicol>, 26:27-30.
Sparkman, O, D, Penton, Z., Fulton, G., 2011, Gas Chromatography and mass spectrometry : a practical guide, Elsivier.
Seok,LD,Shin, HS, and Kang, BK, Systematic Analysis of Stimulants and Narcotic Analgesics by Gas Chromatography with Nitrogen Specific Detection and Mass Spectrometry, J. Anal. Toxicol., 14(3),1990,73-76..
Wijayaputra, N., 2011, Detection of Amphetamine Compounds (MA) in Hair Using SIM GC-MS Method, Thesis, Udayana University, Denpasar.
