Malays. J. Anal. Sci. Volume 29 Number 2 (2025): 1316
Research
Article
Rapid
quantitative detection of saxitoxin using peroxide oxidation derivatization
coupled with fluorescence spectrophotometry
ZiKhang
Chew1, NyukTing Ng1, and Aemi Syazwani Abdul Keyon1,2*
1Department of Chemistry, Faculty of Science,
Universiti Teknologi Malaysia, 81310 Johor Bahru,
Johor, Malaysia
2Centre for Sustainable Nanomaterials, Ibnu Sina
Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, Malaysia
*Corresponding author: aemi@utm.my
Received: 15 September 2024;
Revised: 7 February 2025; Accepted: 3 March 2025; Published: 27 March 2025
Abstract
Often found in North America, Europe, and
Asia, saxitoxin (STX) is a powerful natural marine neurotoxic that is categorized
as a biological weapon. By preventing regular cellular activity, STX has been
shown to cause paralytic shellfish poisoning in both humans and animals..
In the realm of STX analysis, the time required to detect and quantify STX in
water is a crucial concern with implications for public health and regulatory
compliance. Therefore, the peroxide oxidation derivatization coupled with
fluorescence spectrophotometry method for the detection and analysis of STX was
developed in this study. This study was divided into two parts, namely method
optimization and method validation. For optimization part, the optimum
instrumental parameters, excitation and emission spectral bandwidths were fixed
at 5 nm and 20 nm, respectively. While the optimum excitation wavelengths of
oxidized STX was determined as 334 nm. Moreover, the optimum parameters of
peroxide oxidation process, concentration of NaOH and time of reaction were
determined as 0.4 M and 180 s, respectively. For the validation part, the
linear equation for the five-point STX calibration curve (40 – 200 µg/L) was y
= 0.3321x + 5.0021 with a correlation coefficient, R2 of 0.9979.
Based on the linear regression, limit of detection (LOD=3.3 σ/S, with
σ as the standard deviation of calibration curve and S as the slope of
calibration curve) and limit of quantification (LOQ=10 σ/S) were found to
be 11.92 and 36.11 µg/L, respectively, were at par
with the guideline values of recreation water (30 µg/L). The precision and
accuracy results were studied at three concentrations of STX, 50, 100, and 150 µg/L. For precision study, relative standard deviations were
determined in the range of 0.35-1.10% for intra-day precision and 0.51-2.81%
for inter-day precision. For accuracy study, relative
recoveries were determined, ranging from 101-103%. This developed analytical
methods for the STX detection offered these advantages of rapidity
(approximately 4 min), sustainable, high precision, and high accuracy
alternative to conventional methods.
Keywords: Saxitoxin, peroxide
oxidation, fluorescence spectrophotometry, paralytic shellfish poisoning,
analytical eco-scale
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