Development and Validation GC/MS Method for Methamphetamine Analysis in Urine by Miniaturization QuEChERS
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Keywords:
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GC-MS, QuEChERS, Urine, Methamphetamine, Validation
Abstract
This paper explains the development of a quick and easy gas chromatography (GC) approach to identify methamphetamine in urine. This research used gas chromatography with mass spectroscopy and a capillary column TG-5SILMS (5% phenyl methyl siloxane, 30 m x 0.32 x 25 m). The carrier gas flow rate was set at 1.0 mL/minute, the temperature inlet and detector had been set at 300°C, and the oven temperature was programmed to initiate at 50°C and held for 1.5 minutes before being raised to 300°C at a rate 40°C/minute and held for 3 minutes. Sample pre-treatment by modification of the QuEChERS method includes using a relatively large amount of inorganic salt, extraction volume and extraction cycle. The optimal conditions for processing a 400 uL urine sample were 160 mg magnesium sulphate, 40 mg sodium chloride, and 400 uL acetonitrile for organic solvent. According to the validation test, the detection limit for methamphetamine was 0.36 ug/mL; the quantitation limit was 1.09 ug/mL, and the calibration curve followed the regression line. y=1.0489x-3.7914, coefficient (r) was 0.9973. The recovery of the analyte spiked into urine at 5, 7 and 9 ug/mL on average was 100.5±2.33% for intraday dan 93.3±7.21% for interday. The precision was excellent, with an average coefficient of variation of 2.31%. The procedure was applied to four urine samples from drug users and the first abuser (25.51 ug/mL), the second abuser (15.05 ug/mL), the third abuser (17.72 ug/mL) and the last abuser (3.08 ug/mL) were all satisfactorily quantitated.
References
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Seidi, S., M. Tajik, M. Baharfar, and M. Rezazadeh (2019). Micro Solid-phase Extraction (Pipette Tip and Spin Column) and Thin Film Solid-phase Microextraction: Miniaturized Concepts for Chromatographic Analysis. TrAC Trends in Analytical Chemistry, 118; 810–827
Stevens, J. and D. Jones (2010). QuEChERS 101: The Basics and Beyond. Agil. Technol.
Volkow, N. D., J. S. Fowler, G. J. Wang, E. Shumay, F. Telang, P. K. Thanos, and D. Alexoff (2010). Distribution and Pharmacokinetics of Methamphetamine in the Human Body: Clinical Implications. PloS one, 5(12); 15269
Westland, J. L. and F. L. Dorman (2013). QuEChERS Extraction Of Benzodiazepines In Biological Matrices. Journal of Pharmaceutical Analysis, 3(6); 509–517
Woźniak, M. K., M. Wiergowski, J. Aszyk, P. Kubica, J. Namieśnik, and M. Biziuk (2018). Application of Gas Chromatography–tandem Mass Spectrometry for the Determination of Amphetamine type Stimulants in Blood and Urine. Journal of Pharmaceutical and Biomedical Analysis, 148; 58–64
Anastassiades, M., S. J. Lehotay, D. Štajnbaher, and F. J. Schenck (2003). Fast And Easy Multiresidue Method Employing Acetonitrile Extraction/partitioning and “dispersive Solid-phase Extraction” For the Determination of Pesticide Residues in Produce. Journal of AOAC International, 86(2); 412–431
Asl, S., M. Khodayar, Z. Mousavi, and M. Akhgari (2017). Methadone Extraction by Modified Quechers and Liquid-Liquid Extraction from Post-mortem Urine by GC-MS. Journal Medical Toxicology Clinic Forensic Medicine, 3; 1–4
Campêlo, J. d. M., T. B. Rodrigues, J. L. Costa, and J. M. Santos (2021). Optimization of QuEChERS Extraction for Detection and Quantification of 20 Antidepressants in Postmortem Blood Samples by LC-MS/MS. Forensic Science International, 319; 110660
Carasek, E., L. Morés, and R. D. Huelsmann (2022). Disposable Pipette Extraction: a Critical Review of Concepts, Applications, and Directions. Analytica Chimica Acta, 1192; 339383
Correia-Sá, L., S. Norberto, C. Delerue-Matos, C. Calhau, and V. F. Domingues (2018). Micro QuEChERS Extraction Coupled to GC–MS for a Fast Determination of Bisphenol A in Human Urine. Journal of Chromatography B, 1072; 9–16
Cruickshank, C. C. and K. R. Dyer (2009). A Review of the Clinical Pharmacology of Methamphetamine. Addiction, 104(7); 1085–1099
Dalimunthe, N. A., Z. Alfian, B. Wijosentono, and E. Eddyanto (2019). Analisa Kualitatif Kandungan Senyawa Metamfetamin Dalam Rambut Pengguna Sabu-Sabu Dengan Metode Ekstraksi Fase Padat (SPE) Menggunakan Adsorben Zeolit Serulla. Ready Star, 2(1); 130–134 (In Indonesia)
Granquist, L., A. Carlsson, S. Jonson, K. Andersson, P. Karlsson, J. Dahlén, and S. Dunne (2019). Optimization of Peak Area Precision of a GC–MS Drug Screening Method Using a Nonparametric Sign Test. Accreditation and Quality Assurance, 24; 215–226
Guideline, I. H. (2019). Bioanalytical Method Validation M10. Draft version, 26
Gujar, A., T. Anderson, D. Cavagnino, and A. Patel (2018). Comparative Analysis of Mass Spectral Matching for Confident Compound Identification Using the Advanced Electron Ionization Source For GC-MS. Thermoscientific, 10598; 1–7
Kaur, G. and S. Sharma (2018). Gas Chromatography-A Brief Review. International Journal of Information and Computing Science, 5; 125–131
Kim, I., J. M. Oyler, E. T. Moolchan, E. J. Cone, and M. A. Huestis (2004). Urinary Pharmacokinetics of Methamphetamine and its Metabolite, Amphetamine Following Controlled Oral Administration to Humans. Therapeutic Drug Monitoring, 26(6); 664–672
Lawal, A., R. C. S. Wong, G. H. Tan, L. B. Abdulra’uf, and A. M. A. Alsharif (2018). Recent Modifications and Validation of QuEChERS-dSPE Coupled to LC–MS and GC–MS Instruments for Determination of Pesticide/agrochemical Residues in Fruits and Vegetables. Journal of Chromatographic Science, 56(7); 656–669
Maggira, M. and V. Samanidou (2018). QuEChERS: the Dispersive Methodology Approach for Complex Matrices. Journal Chromatography Separation Technology, 9; 1–3
Matsuta, S., K. Nakanishi, A. Miki, K. Zaitsu, N. Shima, T. Kamata, H. Nishioka, M. Katagi, M. Tatsuno, and K. Tsuboi (2013). Development of a Simple one-pot Extraction Method for Various Drugs and Metabolites of Forensic Interest in Blood by Modifying the QuEChERS Method. Forensic Science International, 232(1-3); 40–45
National, N. A. (2019). Press Release of National Narcotics Agency: “Make Drugs Our Common Enemy. 1-39. National Narcotics Agency
Numbers, U. P. (2017). A Modified QuEChERS Approach for the Extraction of Common Prescription and Illicit Drugs from Liver Prior to LC/MS-MS Analysis. March; 30–32
Orfanidis, A., A. Krokos, O. Mastrogianni, H. Gika, N. Raikos, and G. Theodoridis (2022). Development and Validation of a Single Step GC/MS Method for the Determination of 41 Drugs and Drugs of Abuse in Postmortem Blood. Forensic Sciences, 2(3); 473–491
Perestrelo, R., P. Silva, P. Porto Figueira, J. A. Pereira, C. Silva, S. Medina, and J. S. Câmara (2019). QuEChERS-Fundamentals, Relevant Improvements, Applications and Future Trends. Analytica Chimica Acta, 1070; 1–28
Pouliopoulos, A., E. Tsakelidou, A. Krokos, H. Gika, G. Theodoridis, and N. Raikos (2018). Quantification of 15 Psychotropic Drugs in Serum and Postmortem Blood Samples After a Modified Mini-QuEChERS by UHPLC–MS-MS. Journal of Analytical Toxicology, 42(5); 337–345
Rothman, R. B., M. H. Baumann, C. M. Dersch, D. V. Romero, K. C. Rice, F. I. Carroll, and J. S. Partilla (2001). Amphetamine-type Central Nervous System Stimulants Release Norepinephrine More Potently Than They Release Dopamine and Serotonin. Synapse, 39(1); 32–41
Samuels, P. (2015). Pearson Correlation. April. Pearson Correlation Schmidt, M. L. and N. H. Snow (2016). Making the Case for QuEChERS-Gas Chromatography of Drugs. TrAC Trends in Analytical Chemistry, 75; 49–56
Seidi, S., M. Tajik, M. Baharfar, and M. Rezazadeh (2019). Micro Solid-phase Extraction (Pipette Tip and Spin Column) and Thin Film Solid-phase Microextraction: Miniaturized Concepts for Chromatographic Analysis. TrAC Trends in Analytical Chemistry, 118; 810–827
Stevens, J. and D. Jones (2010). QuEChERS 101: The Basics and Beyond. Agil. Technol.
Volkow, N. D., J. S. Fowler, G. J. Wang, E. Shumay, F. Telang, P. K. Thanos, and D. Alexoff (2010). Distribution and Pharmacokinetics of Methamphetamine in the Human Body: Clinical Implications. PloS one, 5(12); 15269
Westland, J. L. and F. L. Dorman (2013). QuEChERS Extraction Of Benzodiazepines In Biological Matrices. Journal of Pharmaceutical Analysis, 3(6); 509–517
Woźniak, M. K., M. Wiergowski, J. Aszyk, P. Kubica, J. Namieśnik, and M. Biziuk (2018). Application of Gas Chromatography–tandem Mass Spectrometry for the Determination of Amphetamine type Stimulants in Blood and Urine. Journal of Pharmaceutical and Biomedical Analysis, 148; 58–64
Authors
Aulia, S., Primaharinastiti, R. ., & Purwanto, D. A. . (2023). Development and Validation GC/MS Method for Methamphetamine Analysis in Urine by Miniaturization QuEChERS. Science and Technology Indonesia, 8(3), 451–460. https://doi.org/10.26554/sti.2023.8.3.451-460
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