Malaysian Journal of Analytical Sciences, Vol 27 No 3 (2023): 600 - 611

 

IN-SYRINGE DISPERSIVE SOLID PHASE MICROEXTRACTION FOR THE DETERMINATION OF ORGANOPHOSPHORUS PESTICIDE RESIDUES IN VEGETABLES

 

(Pengestrakan Mikro Fasa Pepejal Secara Penyerakan dalam Picagari bagi Penentuan Sisa Racun Jenis Organofosforus dalam Sayur-Sayuran)

 

Hairul Nizwan Manap1, Faizah Binti Mohammad Yunus1, Nur Nadhirah Mohamad Zain2, Noorfatimah Yahaya2, Hemavathy Surikumaran3, Kumuthini Chandrasekaram4,6, Kavirajaa Pandian Sambasevam5,7, Muggundha Raoov1,4*

 

1Department of Chemistry, Faculty of Science,

University of Malaya, 50603 Kuala Lumpur, Malaysia.

2Department of Toxicology, Advanced Medical & Dental Institute,

Universiti Sains Malaysia, 13200 Kepala Batas, Pulau Pinang, Malaysia

3Faculty of Bioeconomic and Health Sciences,

Universiti Geomatika Malaysia, 54200 Kuala Lumpur, Malaysia

4Universiti Malaya Centre for Ionic Liquids (UMCIL), Department of Chemistry,

Faculty of Science, Universiti Malaya, Kuala Lumpur, Malaysia

5Advanced Materials for Environmental Remediation (AMER), Faculty of Applied Sciences,

Universiti Teknologi MARA, Negeri Sembilan Branch, Kuala Pilah Campus, Kuala Pilah, Malaysia

6Research Services Division (BPP, Institute of Research Management & Services (IPPP),

University of Malaya, 50603 Kuala Lumpur, Malaysia

7Electrochemical Materi and Sensor (EMaS) Research Group,

Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

 

*Corresponding author: muggundha@um.edu.my

 

Received: 29 December 2022; Accepted: 20 May 2023; Published:  23 June 2023

 

Abstract

In-syringe dispersive solid-phase microextraction with activated carbon as adsorbent was successfully developed to determine organophosphorus pesticide (OPP) residues in vegetable samples and the analytes were detected using gas chromatography-flame photometric detector (GC-FPD). Under optimized conditions (6 mg of activated carbon in 10 mL sample volume with 3 min extraction time and desorption with 300 µL of acetone), activated carbon was proven to be an effective adsorbent for the organophosphorus pesticide residues in vegetable samples with a satisfactory percentage recovery achieved from 81.46 to 108.93%. All the studied analytes showed good linearity in the range of 10 to 500 µg kg-1 and the correlation of determination (R2) was from 0.9962 to 0.9985. The LODs obtained were from 0.39 to 0.84 µg kg-1, and LOQs were from 1.18 to 2.56 µg kg-1. This method gives precision values for both intra- and inter-day within accepted variable limits (<15 % of RSD). The in-syringe dispersive solid-phase microextraction managed to eliminate the centrifugation process, reduce chemical consumption during extraction, and additionally speed up the extraction process, making it more efficient. This developed method can be applied to real samples such as vegetables and fruit juices as well as tap, river, or ground water analysis for the determination of OPPs.

 

Keywords: organophosphorus pesticide, in-syringe dispersive solid phase microextraction, gas chromatography-flame photometric detector

 

Abstrak

Pengekstrakan mikro fasa pepejal dalam picagari dengan menggunakan karbon aktif sebagai penyerap telah berjaya dibangunkan untuk menentukan sisa racun perosak jenis organofosforus (OPP) dalam sampel sayur-sayuran dan analisis telah dikesan dengan menggunakan peralatan analisis kromatografi gas – pengesan fotometrik nyalaan (GC-FPD). Di bawah keadaan yang dioptimumkan (6 mg karbon aktif dalam isipadu sampel 10 mL dengan masa pengekstrakan selama 3 minit dan diserap dengan 300 μL aseton), karbon aktif terbukti sebagai penyerap berkesan bagi sisa racun perosak organofosforus dalam sampel sayur-sayuran berdasarkan peratusan pengesanan semula yang dicapai dari 81.5 hingga 108.9%. Semua analit yang dikaji menunjukkan garis lurus yang baik dalam julat 10 hingga 500 μg kg-1 dan memberikan korelasi penentuan (R2) dari 0.9962 hingga 0.9985. Had pengesanan yang di dapati adalah dari 0.39 hingga 0.84 μg kg-1, dan had pengkuantitian adalah dari 1.18 hingga 2.56 μg kg-1. Kaedah ini memberi nilai ketepatan pada kedua-dua intra dan antara hari dalam sisihan piawai relatif (RSD) yang diterima (<15% daripada RSD). Pengestrakan mikro fasa pepejal secara penyerakan dalam picagari berjaya mengelakkan proses pengemparan, mengurangkan penggunaan bahan kimia dalam proses pengekstrakan dan juga proses pengekstrakan menjadi lebih pantas dan lebih cekap. Kaedah yang dibangunkan ini boleh digunakan untuk sampel sebenar seperti sayur-sayuran, jus buah-buahan dan juga sesuai untuk analisis air paip, air sungai dan air tanah untuk penentuan sisa racun perosak organofosforus.

 

Kata kunci: perosak jenis organofosforus, pengekstrakan mikro fasa pepejal dalam picagari, kromatografi gas – pengesan fotometrik nyalaan

 

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