Sains Malaysiana 46(1)(2017): 149–156

http://dx.doi.org/10.17576/jsm-2017-4601-19

Impurity Profiling of Amphetamine and Methamphetamine Using Gas Chromatography Mass Spectrometry (GCMS) Harmonised Methods

(Pemprofilan Bendasing Amfetamin dan Metamfetamin Menggunakan Kaedah Pengharmonian Analisis Kromatografi Gas Spektrometri (GCMS))

WAN NUR SYUHAILA MAT DESA* & DZULKIFLEE ISMAIL

Forensic Science Programme, School of Health Sciences, Universiti Sains Malaysia

16150 Kubang Kerian, Kelantan Darul Naim, Malaysia

Received: 23 February 2016/Accepted: 9 May 2016

ABSTRACT

Impurity profiling of drug seizures is a scientific approach employed to understand drug trafficking networks thus has becoming increasingly important in criminal investigation. This paper presents the feasibility of using the Collaborative Harmonisation of Methods for the Profiling of Amphetamine Type Stimulants (CHAMP) established by the European Commission authority for impurity profiling of amphetamine and methamphetamine samples. Both drugs were analysed using similar extraction procedure and analytical conditions. The impurities were extracted from an alkaline buffer solution (pH8.1) using toluene prior to gas chromatography-mass spectrometry (GC-MS) analyses. The results showed that the reproducibility of the method for detecting amphetamine and methamphetamine ranged between 7.4-8.9 and 6.2-8.4 %RSD, respectively. Identification of impurities was performed by referencing against the available MS databases as well as to previous reported impurity profiling studies. Phenyl-2-propanone (P2P), also known as benzyl-methyl-ketone (BMK), as well as other specific impurities such as 4-methyl-5-phenylpyrimidine, bis-(1-phynelisopropyl) amine, N-formylamphetamine and N,N-di (b-phenylisopropyl) amines were identified in the amphetamine samples, indicating Leuckart’s pathway as the route of synthesis. Because P2P was also detected in the methamphetamine samples, the possible route of synthesis of the methamphetamine samples being Leuckart’s, nitrostyrene synthesis or reductive amination could not be ruled out.

Keywords: Amphetamine; chromatographic profiles; impurities; mass spectrum; methamphetamine

ABSTRAK

Pemprofilan bendasing bagi rampasan dadah merupakan pendekatan saintifik yang diguna pakai bagi memahami jaringan penyeludupan dadah yang menjadi semakin penting dalam penyiasatan jenayah. Kertas ini membentangkan kebolehlaksanaan Kaedah Pengharmonian Kolaboratif untuk Pemprofilan Amfetamin (CHAMP) yang diwujudkan oleh Suruhanjaya Eropah bagi pemprofilan dadah amfetamin dan metamfetamin. Sampel telah dianalisa dengan melalui proses pengekstrakan dan analisis yang sama. Pengekstrakan bendasing dilakukan menggunakan larutan penimbal beralkali (pH8.1) dengan toluen sebelum analisis kromatografi gas-spektrometri (GC-MS) dijalankan. Kebolehulangan pengesanan yang direkodkan bagi amfetamin dan metamfetamin masing-masing ialah 7.4-8.9 dan 6.2-8.4% RSD. Pengenalpastian bendasing telah dilakukan dengan merujuk kepada pengkalan data MS dan kajian yang telah dijalankan sebelum ini. Fenil-2-propanon(P2P) atau juga dikenali sebagai benzil-metil-keton (BMK) telah dikenal pasti dalam sampel amfetamin selain bendasing seperti 4-metil-5-fenilpirimidina,bis-(1-fenilisopropil) amina, N-formilamfetamina dan N, N-di (b-isopropil) amina yang menunjukkan penggunaan kaedah sintesis Leuckart. P2P telah dikesan di dalam sampel metamfetamin yang menunjukkan laluan sintesis bagi dadah ini adalah berkemungkinan Leuckart, nitrostirena atau reduktif aminasi.

Kata kunci: Amfetamin; bendasing; metamfetamin; pemprofilan kromatografi; spektrum jisim

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*Corresponding author; email: wannurs@usm.my