Malaysian Journal of Analytical Sciences, Vol 28 No 2 (2024): 277 - 289

 

ENRICHED SILICA FROM OIL PALM BIOMASS FOR MAGNETIC SOLID PHASE EXTRACTION OF ORGANOCHLORINE PESTICIDE: CHARACTERIZATION AND METHOD DEVELOPMENT

 

(Silika yang Diperkayakan daripada Biomas Kelapa Sawit untuk Pengekstrakan Fasa Pepejal Magnetik Organoklorin Racun Serangga: Ciri dan Pembangunan Kaedah)

 

Nur Husna Zainal Abidin1, Amir Hisyam Othman1, Wan Nazihah Wan Ibrahim1*, Nordiana Suhada Mohammad Tahirudin 1,2 , Nor Suhaila Mohamad Hanapi1, and Nursyamsyila Mat Hadzir1

 

1Faculty of Applied Sciences, 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: 10 September 2023; Accepted: 12 March 2024; Published:  29 April 2024

 

 

Abstract

This study focused on preparing magnetic silica bio-sorbent made from oil palm fronds and developing methods for analyzing trace amounts of organochlorine pesticides, including Aldrin, Dieldrin, and Heptachlor. The bio-sorbent, namely Fe3O4@SiO2, was prepared through the sol-gel method by combining silica particles derived from oil palm fronds with commercial ferrous (II) oxide. The physical and chemical properties of the bio-sorbents were analyzed using ATR-FTIR, FESEM, EDX, and XRD. According to ATR-FTIR, the bio-sorbent contained absorption bands at 1100 cm-1 and 500-600 cm-1, indicating the functional groups of Si-O and Fe-O. FESEM and EDX studies show the particles have a rough and irregular surface morphology that is composed of 63.9% oxygen, 16.97% silica, and 19.04% ferrous atomic weight. Meanwhile, XRD analysis confirmed that the bio-sorbent was composed of face-centered cubic Fe3O4 and amorphous SiO2, with multiple peaks appearing at 2θ = 22.978 (101), 30.20 (220), 35.60 (311), and 57.50. A magnetic solid-phase extraction method using the synthesized bio-sorbent was developed prior to gas chromatography-mass spectrometry analysis of the selected OCPs. The optimal extraction conditions were determined via one variable at a time (OVAT) and resulted as follows: extraction time, 5 min; desorption solvent, ethyl acetate; desorption time, 5 min; mass of sorbent, 40 mg. The analytical performance of the method was evaluated under these conditions, with a detection limit of 0.1-0.53 mg/L and an extraction recovery of 80-92%. Several linear ranges were obtained for Heptachlor, Aldrin, and Dieldrin, including 0.6-1.8, 0.1-0.3, and 0.2-0.6 mg/L, respectively. The effectiveness of the bio-sorbent was proven by removing pesticides from actual paddy water samples, with calibration curves showing linearity over a wide range of values. The intra- and inter-day precisions were 0.50-1.86% and 0.69-2.54%, respectively.

 

Keywords: bio-sorbent magnetic silica, organochlorine, paddy water samples, magnetic solid phase extraction

 

Abstrak

Kajian ini bertujuan untuk menghasilkan biosorbent silika magnetik daripada pelepah kelapa sawit dan membangunkan kaedah untuk menganalisis jumlah jejak racun serangga organoklorin seperti Heptachlor, Aldrin, dan Dieldrin. Bio-sorben iaitu Fe3O4-SiO2 telah disediakan melalui kaedah sol-gel dengan menggabungkan zarah silika yang diperolehi daripada pelepah kelapa sawit dengan ferus (II) oksida komersial. Sifat fizikal dan kimia bio-sorben telah dianalisis menggunakan ATR-FTIR, FESEM, EDX, dan XRD. Menurut ATR-FTIR, bio-sorben mengandungi julat penyerapan pada 1100 cm-1 dan 500-600 cm-1, yang menunjukkan kumpulan fungsi Si-O dan Fe-O. Kajian FESEM dan EDX menunjukkan bahawa partikel mempunyai morfologi permukaan yang kasar dan tidak teratur yang terdiri daripada 63.9% oksigen, 16.97% silika, dan 19.04% berat atom ferus. Sementara itu, analisis XRD mengesahkan bahawa bio-sorben terdiri daripada Fe3O4 kubik berpusat muka dan SiO2 amorfus, dengan pelbagai puncak yang muncul pada 2θ = 22.978 (101), 30.20 (220), 35.60 (311), dan 57.50. Pembangunan kaedah pengekstrakan fasa pepejal magnet dengan menggunakan bio-sorben yang disintesis telah dijalankan diikuti analisis oleh kromatografi gas spektrometri jisim (GC-MS) daripada OCP yang terpilih. Keadaan pengekstrakan optimum ditentukan melalui satu parameter pada satu masa dan hasilnya seperti berikut: masa pengekstrakan 5 min; pelarut desorpsi, etil esitat; masa desorpsi, minit, dan sorbent jisim 40 mg. Prestasi analisis kaedah dinilai di bawah keadaan ini, dengan had pengesanan 0.1-0.53 mg/L dan pemulihan pengekstrakan 80-92%. Beberapa julat linear telah diperolehi untukHeptachlor, Aldrin dan Dieldrin, termasuk 0.6-1.8, 0.1-0.3, dan 0.2-0.6 mg/L masing-masing. Keberkesanan biosorben telah dibuktikan dengan mengeluarkan racun perosak daripada sampel air padi sebenar, dengan lengkung penentukuran menunjukkan kelinearan ke atas julat nilai yang luas.Ketepatan dalam dan antara hari ditemui dalam julat 0.50-1.86% dan 0.69-2.54%, masing-masing.

 

Kata kunci: bio-sorben silika magnet, organoklorin, sampel air padi, pengekstrakan fasa pepejal magnet

 

 

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