Malaysian Journal of Analytical Sciences, Vol 28 No 2 (2024): 441 - 460

 

PRE-CONCENTRATION OF ORGANOCHLORINE PESTICIDES USING MICRO-SOLID PHASE EXTRACTION BASED ON BIO-SORBENT ALGINATE-SILICA BEADS DERIVED FROM OIL PALM FROND

 

(Pra-Kepekatan Racun Organoklorin Menggunakan Pengekstraksi Fasa Mikro-Pepejal Berasaskan Bio-sorben Alginat-Silika Komposit yang Diperoleh daripada Daun Pelepah Kelapa Sawit)

 

Azreen Asyikin Mhd Kamal1, Siti Nur Afiqah Binti Mahazan1, Nur Husna Zainal Abidin1, Fariesha Farha Ramli1,2, and Wan Nazihah Wan Ibrahim1*

 

1Faculty of Applied Science, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

2Faculty of Applied Science, Universiti Teknologi MARA, Perak Branch, Tapah Campus, 35400, Perak

 

*Corresponding author: wannazihah@uitm.edu.my

 

 

Received: 27 September 2023; Accepted: 16 January 2024; Published:  29 April 2024

 

 

Abstract

This study focuses on the extraction of organochlorine pesticides (OCPs) contained in environmental water samples by using encapsulated alginate-silica (Alg-SiO2) composite beads. The composite beads were made by ionic crosslinking interaction between polymeric alginate and silica particles derived from oil palm fronds and were characterized by ATR-FTIR, FESEM, and EDX to study their chemical and physical properties. The Alg-SiO2 composite beads were then used as the sorbent material for the micro-solid phase extraction ( -SPE) to extract OCPs from aqueous samples. Optimization of method development for extraction of targeted analytes (heptachlor, aldrin, and dieldrin) was done by varying the extraction time, extraction solvent, desorption time, and sorbent mass before the gas chromatography-mass spectrometry analysis. Analytical figures of merit for -SPE were calculated under the optimized extraction conditions. Under the optimum conditions of 50 mg of sorbent extracted for 5 mins and desorbed using n-hexane for 7 mins, good linearity was achieved based on the data from method validation, linear ranges of 1–10 mg/L for heptachlor, 0.1–1.0 mg/L for aldrin, and 0.2–1.4 mg/L for dieldrin, with a limit of detection of 0.09–0.85 mg/L. The proposed method was successfully applied to determine organochlorine pesticides in paddy water samples. The wide range of the calibration curves was linear, and the coefficients of regression were all around 0.979-0.993. The recoveries were obtained in a satisfactory range of 82-98%, and the precision RSD value was in the range of 0.19-4.52%.

 

Keywords: alginate, silica sorbent, organochlorine, oil palm, micro solid phase extraction

 

Abstrak

Kajian ini memfokuskan kepada pengekstrakan racun perosak organoklorin (OCP) yang terkandung dalam sampel air persekitaran dengan menggunakan kapsulan manik komposit alginat-silika (Alg-SiO2). Manik komposit dibuat melalui interaksi pertautan silang ion antara polimer alginat dan zarah silika yang diperoleh daripada pelepah kelapa sawit, dan dicirikan oleh ATR-FTIR, FESEM, dan EDX untuk mengkaji sifat kimia dan fizikalnya. Manik komposit Alg-SiO2 kemudiannya digunakan sebagai bahan penjerap untuk pengekstrakan fasa pepejal mikro (μ-SPE) untuk mengekstrak OCP daripada sampel akueus. Pengoptimuman pembangunan kaedah untuk pengekstrakan analit yang disasarkan (heptaklor, aldrin, dan dieldrin) dilakukan dengan mempelbagaikan masa pengekstrakan, pelarut pengekstrakan, masa nyahjerapan dan jisim penjerap sebelum analisis spektrometer jisim gas kromatografi. Angka analisis merit untuk μ-SPE dikira di bawah keadaan pengekstrakan yang dioptimumkan. Di bawah keadaan optimum 50 mg penjerap yang diekstrak selama 5 min dan nyahjerap menggunakan n-heksana selama 7 min telah menghasilkan julat linear yang baik. Berdasarkan data yang diperoleh daripada pengesahan kaedah, julat linear 1–10 mg/L untuk heptaklor, 0.1–1.0 mg/L untuk aldrin, dan 0.2–1.4 mg/L untuk dieldrin, dengan had pengesanan 0.09–0.85 mg/L. Kaedah yang dicadangkan telah berjaya digunakan untuk menentukan racun perosak organoklorin dalam sampel air padi. Julat luas keluk penentukuran adalah linear, dan pekali regresi adalah sekitar 0.979-0.993. Pemulihan diperolehi dalam julat yang memuaskan iaitu 82-98% dan nilai ketepatan RSD dalam julat 0.19-4.52%.

 

Kata kunci: alginat, silika sorben, organoklorin, kelapa sawit, pengekstraksi fasa mikro-pepejal


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