Research Article

Development of qualitative GC MS method for simultaneous identification of PM-CCM a modified illicit drugs preparation and its modern-day application in drug-facilitated crimes

Bhagat Singh*, Satish R Nailkar, Chetansen A Bhadkambekar, Suneel Prajapati and Sukhminder Kaur

Published: 28 March, 2023 | Volume 7 - Issue 1 | Pages: 004-010

Prescriptions for psychoactive substances such as Pregabalin, Methamphetamine, Caffeine, Clonazepam and Mirtazapine (PM-CCM) are common in the treatment of a variety of disorders. Indeed, the PM-CCM has been used in different therapeutic areas, including insomnia, anxiety, seizure disorders, etc. Unfortunately, these psychoactive substances are present in the illegal street market, leading to a lot of drug abuse among some addicted users, road insecurity and suicide. Hence, it has become essential to validate and develop a rapid and effective method to analyze the PM-CCM, a modified illicit drug, for drug abuse in the forensic sciences. A simple, rapid, specific and sensitive Gas Chromatography-Mass Spectrometry(GC-MS) method has been developed for the identification of Pregabalin, Methamphetamine, Caffeine, Clonazepam and Mirtazapine (PM-CCM) in forensic exhibits. At room temperature, the sample was ultrasonicated for 5 minutes before being extracted with methanol. A highly precise auto-injector is used to inject a very small quantity of samples for analysis. Helium is used as a carrier gas with a flow rate of 1 ml/min. The separation of PM-CCM was performed on SH-RXi-5 MS, ID.25 mm, film thickness. 25 µm, length of 30 m column. The constituents of PM-CCM were identified by the mass-to-charge ratio (m/z ratio) of fragments of the parent compound by comparing them with the NIST-17 MS Library. Separation and identification of PM-CCM were achieved within a 15-minute run. The proposed method has been successfully used for the routine analysis of PM-CCM in complex illicit drug preparations and in forensic exhibits as well. The application of above discussed qualitative analysis method and screening of PM-CCM, modified illicit drug samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples.


Read Full Article HTML DOI: 10.29328/journal.jfsr.1001043 Cite this Article Read Full Article PDF


GC-MS; PM-CCM; Pregabalin; Methamphetamine; Mirtazepine; Clonazepam; Caffeine


  1. Aberhausen UN. United Nations Office on Drugs and Crime. Resolutions and Decisions. 2018. unodc.org/unodc/en/commissions/CND/Resolutions_Decisions/Resolutions-Decisions.
  2. Azimi S, Docoslis A. Recent Advances in the Use of Surface-Enhanced Raman Scattering for Illicit Drug Detection. Sensors (Basel). 2022 May 20;22(10):3877. doi: 10.3390/s22103877. PMID: 35632286; PMCID: PMC9143835.
  3. Crowley R, Kirschner N, Dunn AS, Bornstein SS; Health and Public Policy Committee of the American College of Physicians; Abraham G, Bush JF, Gantzer HE, Henry T, Kane GC, Lenchus JD, Li JM, McCandless BM, Candler SG. Health and Public Policy to Facilitate Effective Prevention and Treatment of Substance Use Disorders Involving Illicit and Prescription Drugs: An American College of Physicians Position Paper. Ann Intern Med. 2017 May 16;166(10):733-736. doi: 10.7326/M16-2953. Epub 2017 Mar 28. PMID: 28346947.
  4. Joye T. Bararpour N, Augsburger M, Boutrel B, Thomas A. In situmetabolomic changes in rat hippocampus after acute cocaine administration.  J. Mass Spectrom. 2017; 437: 87–91; 10.1016/j.ijms. 2017;12:001.
  5. Vearrier L. The value of harm reduction for injection drug use: A clinical and public health ethics analysis. Dis Mon. 2019 May;65(5):119-141. doi: 10.1016/j.disamonth.2018.12.002. Epub 2018 Dec 29. PMID: 30600096.
  6. Zaccara G, Gangemi P, Perucca P, Specchio L. The adverse event profile of pregabalin: a systematic review and meta-analysis of randomized controlled trials. Epilepsia. 2011 Apr;52(4):826-36. doi: 10.1111/j.1528-1167.2010.02966.x. Epub 2011 Feb 14. PMID: 21320112.
  7. Pfizer Canada Inc. Lyrica® Product Monograph. December 6, 2016. http://www.pfizer.ca/sites/g/files/g10028126/f/201612/LYRICA_DC_PM_198215_6Dec2016_E.pdf
  8. Hložek T, Uttl L, Kadeřábek L, Balíková M, Lhotková E, Horsley RR, Nováková P, Šíchová K, Štefková K, Tylš F, Kuchař M, Páleníček T. Pharmacokinetic and behavioural profile of THC, CBD, and THC+CBD combination after pulmonary, oral, and subcutaneous administration in rats and confirmation of conversion in vivo of CBD to THC. Eur Neuropsychopharmacol. 2017 Dec;27(12):1223-1237. doi: 10.1016/j.euroneuro.2017.10.037. Epub 2017 Nov 10. PMID: 29129557.
  9. Donald JA. Medicinal Chemistry and Drug discovery (6th edn) Wiley, New Jersey. 2003; 312-313.
  10. Warner G, Figgitt DP. Pregabalin: as adjunctive treatment of partial seizures. CNS Drugs. 2005;19(3):265-72; discussion 273-4. doi: 10.2165/00023210-200519030-00007. PMID: 15740180.
  11. Fiorentin TR, Krotulski AJ, Martin DM, Browne T, Triplett J, Conti T, Logan BK. Detection of Cutting Agents in Drug-Positive Seized Exhibits within the United States. J Forensic Sci. 2019 May;64(3):888-896. doi: 10.1111/1556-4029.13968. Epub 2018 Nov 28. PMID: 30485426.
  12. Clarke’s analysis of drugs and poisons, 3rd Eds. AC Moffat, MD Osselton and B Widdop. Pharmaceutical Press, London (UK). 2003; ISBN 085369 473 7.
  13. Assemat G, Balayssac S, Gerdova A, Gilard V, Caillet C, Williamson D, Malet-Martino M. Benchtop low-field 1H Nuclear Magnetic Resonance for detecting falsified medicines. Talanta. 2019 May 1;196:163-173. doi: 10.1016/j.talanta.2018.12.005. Epub 2018 Dec 7. PMID: 30683346.
  14. Burns NK, Theakstone AG, Zhu H, O'Dell LA, Pearson JR, Ashton TD, Pfeffer FM, Conlan XA. The identification of synthetic cannabinoids surface coated on herbal substrates using solid-state nuclear magnetic resonance spectroscopy. Anal Chim Acta. 2020 Apr 1;1104:105-109. doi: 10.1016/j.aca.2019.12.051. Epub 2020 Jan 21. PMID: 32106940.
  15. Seema A, Jeeja P, Ashish J. Development and Validation of HPLC Method for Estimation of Pregabalin in Bulk & Capsule Dosage Form. Pharm Anal Acta. 2016; 7: 492. doi:10.4172/2153-2435.1000492
  16. Gujral RS, Haque SM, Shanker P. Development and Validation of Pregabalin in Bulk, Pharmaceutical Formulations and in Human Urine Samples by UV Spectrophotometry. Int J Biomed Sci. 2009 Jun;5(2):175-80. PMID: 23675132; PMCID: PMC3614770.
  17. Patil DD, Patil MS, Wani YB. Spectrophotometric method for pregabalin determination: An experimental design approach for method development. Jour. of the Associ. of Arab Unive. for Bas. and Appl. Sci. 2018; 21:(21); 31-37.
  18. Mandal U, Sarkar AK, Gowda KV, Agarwal S, Bose A, Bhaumik U, Ghosh D, Pal TK. Determination of Pregabalin in Human Plasma Using LC-MS-MS. Chromatographia 2008; 67(3-4):237-243.
  19. Oertel R, Arenz N, Pietsch J, Kirch W. Simultaneous determination of three anticonvulsants using hydrophilic interaction LC-MS. J Sep Sci. 2009 Jan;32(2):238-43. doi: 10.1002/jssc.200800461. PMID: 19072899.
  20. Vermeij TA, Edelbroek PM. Simultaneous high-performance liquid chromatographic analysis of pregabalin, gabapentin and vigabatrin in human serum by precolumn derivatization with o-phtaldialdehyde and fluorescence detection. J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Oct 25;810(2):297-303. doi: 10.1016/j.jchromb.2004.08.018. PMID: 15380728.
  21. Pavlova V, Petrovska-Jovanovic S. Simultaneous determination of amphetamine, methamphetamine and caffeine in seized tablets by high-performance liquid chromatography.2007;18:157-167
  22. Wen J, Zhang WT, Cao WQ, Li J, Gao FY, Yang N, Fan GR. Enantioselective separation of mirtazapine and its metabolites by capillary electrophoresis with acetonitrile field-amplified sample stacking and its application. Molecules. 2014 Apr 17;19(4):4907-23. doi: 10.3390/molecules19044907. PMID: 24747648; PMCID: PMC6270698.
  23. Labat L, Dallet P, Kummer E, Dubost JP. Spectrophotometric, spectrofluorimetric, HPLC and CZE determination of mirtazapine in pharmaceutical tablets. J Pharm Biomed Anal. 2002; 15;28(2):365-71. doi: 10.1016/s0731-7085(01)00625-2.

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