Citation
Zakaria, Zuliana
(2024)
Validation of inorganic arsenic detection methods using HPLC-ICP-MS and its contamination in market rice in Malaysia.
Masters thesis, Universiti Putra Malaysia.
Abstract
The contamination of inorganic arsenic in rice has become worldwide
concerned due to its associated with cancer effect. The demand for rice has
forced farmers to apply pesticides to meet demand and prevent production
loss especially on a large scale. The pesticide residue, particularly arsenic
pesticides, has the potential to leach into the ground, leading to soil
contamination and the presence of inorganic arsenic (iAs) in paddy seeds.
However, reports on iAs contamination in Malaysian rice remain limited.
Therefore, this study was performed to (1) to validate a reliable analysis for iAs
(As (III), As (V)) in rice by using HPLC-ICP-MS and (2) to determine the iAs
levels in local market rice using the established and validated method. The
sample was grinded, sieved and grinded again until completely transformed to
fine powder before analyse for total Arsenic (As) and iAs. The coefficient of
determination (R2) calculation for the analytes was above 0.99. Also, the
analytes exhibited a limit of detection at 0.002 mg/kg, including the limit of
quantification of 0.005 mg/kg. Calibration standards were established in solution at 1.00μg/kg and 10.00 μg/kg. Recovery studies showed 93.74±6.43
(low concentration), 90.59±3.49 (medium concentration) and 89.63±3.42 (high
concentration). The method was tested on the Food Analysis Performance
Assessment Scheme (FAPAS) Proficiency Test sample and obtained a zscore
of 1.09. Thus, the proposed method proved satisfactory for determining
iAs in rice. The validated method was then tested on 23 rice brand variants,
comprising of 15 imported and 8 domestic rice types. The convenience
sampling approach was used as sampling technique. The recorded data was
between 0.01 mg/kg and 0.102 mg/kg, where brown and coloured rice
displayed 2 to 5 times higher iAs than white rice. None of the samples violated
the Codex Alimentarius Commission (CAC) permissible level (0.20 mg/kg to
0.35 mg/kg) or the maximum permitted limit of European Union (EU) regulation
(0.10 mg/kg to 0.30 mg/kg). In short, this study summarised that the level of
iAs in rice available in the Malaysian market is generally low.
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Additional Metadata
| Item Type: |
Thesis
(Masters)
|
| Subject: |
Environmental Science |
| Subject: |
Analytical Chemistry |
| Subject: |
Food Science |
| Call Number: |
FSTM 2024 12 |
| Chairman Supervisor: |
Ahmad Faizal bin Abdull Razis, PhD |
| Divisions: |
Faculty of Food Science and Technology |
| Keywords: |
Inorganic arsenic; HPLC-ICP-MS; Rice contamination; Malaysia; Pesticide residue; Arsenic speciation; Analytical method validation; Food safety; Brown rice; Codex Alimentarius |
| Depositing User: |
MS. HADIZAH NORDIN
|
| Date Deposited: |
27 Jan 2026 07:19 |
| Last Modified: |
27 Jan 2026 07:21 |
| URI: |
http://psasir.upm.edu.my/id/eprint/122696 |
| Statistic Details: |
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