Page 49 - AJWEP-v22i2

Asian Journal of Water, Environment and Pollution. Vol. 22, No. 2 (2025), pp. 43-50.
doi: 10.36922/ajwep.8196

ORIGINAL RESEARCH ARTICLE

Method validation and its application to gas
chromatography-mass spectrometry analysis of dimethyl

methylphosphonate in OPCW proficiency testing

Faris Rudi 1,2 , Nor Kartini Abu Bakar * , Noor Azilah Mohd Kasim ,
3
1
Mohd Nor Faiz Norrrahim * , and Wan Elyn Amira Wan Adnan 2
4
1 Department of Chemistry, Faculty of Science, Universiti Malaya, Kuala Lumpur, Malaysia
2 Science and Technology Research Institute for Defence (STRIDE), Ministry of Defence, Kajang, Selangor, Malaysia
3 Department of Chemistry and Biology, Center for Defence Foundation Studies, Universiti Pertahanan Nasional Malaysia,
Kem Perdana Sungai Besi, Kuala Lumpur, Malaysia
4 Research Center for Chemical Defence, Universiti Pertahanan Nasional Malaysia, Kem Perdana Sungai Besi, Kuala
Lumpur, Malaysia
*Corresponding authors: Nor Kartini Abu Bakar (kartini@um.edu.my), Mohd Nor Faiz Norrrahim (faiz@upnm.edu.my)

Received: December 25, 2024; Revised: February 15, 2025; Accepted: February 19, 2025; Published online: March 27, 2025

Abstract: The detection and identification of chemical warfare agents (CWAs) are critical to safeguarding global
security, as these toxic substances pose significant threats to human health and the environment. Effective monitoring
and control of CWAs are essential for compliance with the Chemical Weapons Convention. Contamination
of water sources with CWAs or their degradation products can have long-lasting ecological and public health
implications. Dimethyl methylphosphonate (DMMP), a chemical simulant with structural similarities to hazardous
organophosphorus agents, was selected for this study due to its relevance in proficiency testing (PT) and method
validation. Here, we present the development and validation of a gas chromatography-mass spectrometry technique
for the determination of DMMP. The QuEChERS extraction method was utilized to enhance sample preparation
efficiency. The results obtained from the validated method revealed excellent linearity (R² = 0.9998), a low limit of
detection of 0.0167 ppm, and high accuracy and precision, with recovery values between 95.7% and 97.3%, and
low relative standard deviations at 3.5% for intraday and 3.7% for interday. The method was successfully applied
in an Organisation for the Prohibition of Chemical Weapons PT, achieving a recovery value of 95.6% for DMMP.
These results demonstrate the reliability of the method, underscoring its potential for use in international efforts to
monitor and control CWAs, thereby preventing their misuse.

Keywords: Chemical warfare agents; OPCW proficiency testing; QuEChERS; Dimethyl methylphosphonate

1. Introduction concern for global security over a century. The
1
intentional deployment of chlorine gas during World War
Chemical warfare agents (CWAs) include highly toxic I (1914 – 1918) marks the historical commencement of
chemicals and their pre-cursors specifically designed large-scale chemical warfare, with devastating effects.
2
to inflict death, incapacitation, or severe harm upon Throughout the 20 century and into the modern era,
th
individuals. Consequently, their use has been a serious the world has witnessed the terrifying consequences of

Volume 22 Issue 2 (2025) 43 doi: 10.36922/ajwep.8196