Abstract & References Vol 26 No 4 (2022)

Malaysian Journal of Analytical Sciences Vol 26 No 4 (2022): 774 - 787

DETERMINATION OF RESIDUAL XYLAZINE BY GAS CHROMATOGRAPHY IN DRUG-SPIKED BEVERAGES FOR FORENSIC INVESTIGATION

(Penentuan Sisa Xilazin dengan Kromatografi Gas dalam Minuman Ditambah dengan Dadah bagi Penyiasatan Forensik)

Nabeesathul Sumayya Mohamed Sadiq¹, Way Koon Teoh¹, Kasrin Saisahas¹, Apichai Phoncai², Vanitha Kunalan³, Noor Zuhartini Md Muslim¹, Warakorn Limbut^1,4,5, Kah Haw Chang¹, Ahmad Fahmi Lim Abdullah¹*

¹Forensic Science Programme, School of Health Sciences,

Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan, Malaysia

²Division of Health and Applied Sciences, Faculty of Science,

Prince of Songkla University, Hat Yai, Songkhla, 90112, Thailand

³Narcotics Division, Forensic Science Analysis Centre,

Department of Chemistry, Jalan Sultan, 46661 Petaling Jaya, Selangor, Malaysia

⁴Center of Excellence for Trace Analysis and Biosensors (TAB-CoE)

⁵Center of Excellence for Innovation in Chemistry, Faculty of Science

Prince of Songkla University, Hat Yai, Songkhla, 90112, Thailand

*Corresponding author: fahmilim@usm.my

Received: 16 February 2022; Accepted: 15 June 2022; Published: 25 August 2022

Abstract

The utilization of xylazine, a veterinary drug, had recently been reported in drug facilitated crimes (DFC). Victims are incapacitated after consumption of drug-spiked beverages and subsequently exposed to the risk of robbery and sexual assault. In many instances, the suspected drug-spiked beverage samples are available at the scene but the concentration level of xylazine could be very low or restricted by its recoverable amount for forensic testing. To address challenges linked to samples with low or limited recoverable amounts, this study was aimed to establish a laboratory-based gas chromatography method by detecting and quantifying xylazine in drug-spiked beverage samples appearing in liquid, droplet, and dry forms. In this study, a gas chromatography-mass spectroscopy (GC-MS) method was optimized to detect the presence of xylazine, and a gas chromatography-flame ionization detector (GC-FID) method was validated for quantification of the substance. Subsequently, xylazine from four different beverage samples in three different physical forms, simulating the possible forensic settings; were recovered and determined. A validated GC method for the determination and quantification of xylazine within 15 minutes was reported. Limit of detection (LOD) and limit of quantitation (LOQ) were reported at 0.08 µg/mL and 0.26 µg/mL, respectively. Higher recoveries of xylazine were achieved from beverage samples in liquid form (77.2-97.3%) compared to droplet (50.8% – 80.0%) and dry samples (39.8% – 66.9%). This study evidenced that limited volume of leftover beverage samples, and even the dried samples; did not hinder the recovery of the targeted drug. To conclude, a gas chromatographic technique was successfully established for the determination of residual xylazine in drug-spiked beverages that can then provide valuable investigative technique to laboratory analysts and crime scene officers in DFC investigations.

Keywords: forensic science, drug-facilitated crime, xylazine, gas chromatography, drug spiked beverage

Abstrak

Baru-baru ini, penggunaan xilazin, sejenis ubat haiwan, telah dilaporkan dalam jenayah disebabkan dadah (DFC). Mangsa menjadi lemah selepas meminum minuman yang ditambah dengan dadah dan seterusnya terdedah kepada risiko rompakan dan gangguan seksual. Dalam kebanyakan situasi, sampel minuman yang disyaki telah dimasukkan dadah boleh dijumpai di tempat kejadian tetapi tahap kepekatan xilazin berkemungkinan amat rendah atau dibatasi oleh jumlah yang boleh diperolehi semula untuk pengujian forensik. Untuk mengatasi cabaran dalam mengaitkan sampel yang berisipadu rendah atau mempunyai kebolehpulihan yang terhad, kajian ini bertujuan untuk membangunkan satu kaedah kromatografi gas yang berasaskan makmal dengan mengesan dan menentukan kuantiti xilazin dalam sampel minuman yang dimasukkan dadah yang wujud dalam keadaan cecair, titisan dan kering. Dalam kajian ini, satu kaedah kromatografi gas-spektrometri jisim (GC-MS) telah dioptimumkan untuk mengesan kehadiran xilazin dan satu kromatografi gas-pengesanan pengionan nyalaan (GC-FID) telah ditentu-sahkan untuk pengkuantitian sebatian tersebut. Seterusnya, xilazin daripada empat sampel minuman dalam tiga keadaan fizikal berlainan, menyerupai tetapan forensik yang berkemungkinan, telah diperolehi semula dan ditentukan. Satu kaedah GC yang sah bagi penentuan dan penentuan kuantiti xilazin dalam 15 minit telah dilaporkan. Had pengesanan (LOD) dan had pengkuantitian (LOQ) telah dilaporkan masing-masing pada 0.08 μg/mL and 0.26 μg/mL. Xilazin dapat diperoleh semula daripada sampel minuman dalam keadaan cecair dengan peratusan yang lebih tinggi (77.2-97.3%) berbanding dengan sampel titisan (50.8 – 80.0%) dan sampel kering (39.8 – 66.9%). Kajian ini membuktikan bahawa isipadu sampel minuman tertinggal yang terhad dan dalam keadaan kering tidak menghalang perolehan semula dadah yang disasarkan. Kesimpulannya, satu kaedah kromatografi gas telah berjaya dibangunkan untuk menentukan sisa-sisa xilazin dalam minuman yang dimasukkan dadah. Hal ini dapat membantu teknik penyiasatan kepada juruanalisis makmal dan pegawai tempat kejadian dalam penyiasatan DFC.

Kata kunci: sains forensik, jenayah disebabkan dadah, xilazin, kromatografi gas, minuman yang dimasukkan dadah

Graphical Abstract

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