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Sains Malaysiana 41(12)(2012):
1557–1564
Comparison
of Microwave Assisted Acid Digestion Methods for ICP-MS
Determination
of Total Arsenic in Fish Tissue
(Perbandingan Kaedah Penghadaman Asid dengan Bantuan
Mikrogelombangbagi Penentuan Jumlah Arsenik dalam Tisu Ikan Menggunakan ICP-MS)
S. Ghanthimathi*
National Public Health Laboratory, Lot 1853, Kampong Melayu
Sg buloh
47000 Sungai Buloh, Selangor Darul Ehsan, Malaysia
Aminah Abdullah
Pusat Pengajian Sains Kimia dan Teknologi Makanan, Fakulti
Sains dan Teknologi
Universiti Kebangsaan Malaysia,43600 Bangi, Selangor Darul Ehsan, Malaysia
S. Salmijah.
Pusat Pengajian Biosains dan Bioteknologi, Fakulti Sains dan
Teknologi
Universiti Kebangsaan Malaysia,43600 Bangi, Selangor Darul Ehsan, Malaysia
Centre for Public health Science, Queensland Health Forensics and Scientific Services, 39 Kessels Road, Cooper Plains, Qld 4108, Australia
A. Nurul Izzah Institute for Medical Research, Jalan Pahang, 50588 Kuala Lumpur, Malaysia
Diserahkan: 25 Mei 2012 / Diterima: 1 Ogos 2012
ABSTRACT
Fish is one of the most important sources of arsenic exposure in
human diet and the Food Safety and Quality Division, Ministry of Health since
2007 has required routine monitoring of total arsenic in seafoods such as fish.
This study describes an improved extraction method of total arsenic in fish
using microwave assisted acid digestion procedure before being analysed by
inductively coupled plasma mass spectrometry (ICP-MS). The parameters
studied were pre-treatment of sample, digestion temperature, time programme and
the chemicals (HNO3/H2O2) used. Arsenic
contents in fish samples under these conditions were compared using the
standards additions technique. Microwave assisted acid digestion method with a
combination of ultrapure concentrated nitric acid (HNO3) to concentrated
hydrogen peroxide (H2O2) at a ratio of 7
mL: 1 mL, run time of 25 min and digestion temperature of 200°C with no
pre-treatment was found to have recovery of 100.7% as compared to other
digestion procedure where the recovery were 115.5, 111.6 and 101.8%. Validation
using certified reference material (CRM) of fish tissue (DORM-3) showed a recovery
of 101.4 ± 2.5% for total arsenic from the CRM.
Keywords: Arsenic; certified reference material; fish; inductively
coupled plasma mass spectrometry; microwave assisted acid digestion
ABSTRAK
Ikan adalah salah satu daripada sumber yang paling penting bagi
pendedahan arsenik dalam diet manusia dan sejak 2007 Bahagian Keselamatan dan
Kualiti Makanan, Kementerian Kesihatan telah menjalankan pemantauan rutin bagi
jumlah arsenik dalam makanan laut seperti ikan. Kajian ini
menerangkan kaedah pengekstrakan yang diperbaiki bagi jumlah arsenik dalam ikan
dengan menggunakan prosedur penghadaman mikrogelombang dengan bantuan asid
sebelum dianalisis dengan menggunakan spektrometri jisim plasma gandingan
aruhan (ICP-MS). Parameter yang dikaji adalah pra-perlakuan sampel, suhu
penghadaman, program masa dan bahan kimia (HNO3/ H2O2). Kandungan jumlah arsenik dalam sampel ikan dalam keadaan tersebut dibandingkan
dengan menentukan perolehan penambahan bahan piawai jumlah arsenik. Kaedah mikrogelombang dengan bantuan asid dengan gabungan asid nitrik (HNO3)
serta hidrogen peroksida pekat (H2O2) tulen pada
nisbah 7 mL:1 mL dengan masa analisis selama 25 min dan suhu penghadaman 200°C
serta tiada pra-perlakuan sampel, didapati mempunyai nilai perolehan 100.7%
berbandingkan dengan kaedah lain dengan nilai perolehannya adalah 115.5, 111.6
dan 101.8%. Validasi telah dijalankan dengan menggunakan bahan rujukan yang
disahkan atau (CRM) tisu ikan (DORM-3) menunjukkan
perolehan 101.4 ± 2.5% bagi jumlah arsenik dari CRM.
Kata kunci: Arsenik; bahan rujukan yang disahkan; ikan;
mikrogelombang dengan bantuan asid; spektrometri jisim-plasma gandingan aruhan
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*Pengarang
untuk surat-menyurat; email: ghanthimathi@yahoo.com
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