Malaysian
Journal of Analytical Sciences Vol 23 No 3 (2019): 505 - 515
DOI:
10.17576/mjas-2019-2303-15
RAPID SPECTROPHOTOMETRIC METHOD FOR HISTAMINE DETERMINATION IN FISH
USING ALIZARIN RED S AND
METAL
(Kaedah
Spektrofotometri Pantas untuk Penentuan Histamin dalam Ikan Menggunakan Alizarin
Merah S dan Logam)
Miftakhul Jannatin1, Ayu Nabila Izazi
Latjuba1, Sri Wahyuni1, Ganden Supriyanto1,2*, Wan Aini Wan Ibrahim3
1Department of Chemistry, Faculty of Science and Technology
2Laboratory of Sensor and Biosensor, Institute of Tropical Disease
Universitas Airlangga, Jl. Mulyorejo Kampus C UNAIR Surabaya 60115, Indonesia
3Department of Chemistry, Faculty of Science,
Universiti Teknologi
Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia
*Corresponding author: ganden-s@fst.unair.ac.id
Received: 25 October 2017; Accepted: 22 January
2019
Abstract
An analytical method for the determination of histamine
using metals and alizarin red S (ARS) reagents by UV-Visible
spectrophotometry was developed. Cu(II), Co(II) and ARS were used to form colored complex with histamine. The developed method was
used to detect qualitatively and quantitatively the presence of histamine.
Absorbance of Cu(II) and Co(II) complex were measured at a maximum wavelength
of 505.5 and 567 nm, respectively. Optimization of
analytical parameters such as concentration of metals, concentration of ARS,
sample solution pH, and optimum time for complex formation were performed.
Experimental results showed that the optimum concentration of Cu(II) was 50
ppm, 75 ppm ARS, sample solution pH 6, and 15 minutes
optimum time, while the optimum concentration of Co(II) was 125 ppm, ARS was 75
and 50 ppm, sample solution pH 5 and 10 minutes optimum time. Method validation
indicated that the coefficient of variation, limit of detection (LOD) (S/N =3), and limit of quantitation (LOQ = 10S/N) of
Cu(II) were 0.65%, 8.94 ppm, and 29.82 ppm respectively with a sensitivity of
0.0054 ppm and linearity of 0.9959. Accuracy of histamine determination through
Cu-ARS-histamine complex at a concentration of 50,
100, and 150 ppm were 105.7% (RSD = 0.777%, n = 3), 105.06% (RSD = 0.606%, n =
3), and 94.12% (RSD = 0.767%, n = 3), respectively. Meanwhile, the CV, LOD, and
LOQ of Co(II) were 0.28%; 2.58 ppm; and 8.6 ppm respectively with a sensitivity
of 0.0006 ppm and linearity of 0.9965. Accuracy of
histamine determination through Co-ARS-histamine complex at a concentration of
50, 75, and 125 ppm were 98.33%, 95.83%, 93.88%, respectively. The proposed
method was successfully applied to the determination of histamine in a fish sample with quantitative recovery; for Cu(II) complex
(99.23%) and Co(II) complex (102.62%).
Keywords: histamine, metals, Cu(II), Co(II), ARS,
UV-visible spectrophotometry
Abstrak
Kaedah analisis
untuk penentuan histamin menggunakan logam dan reagen alizarin merah S (ARS) telah dibangunkan menggunakan
spektrofotometri ultralembayung-nampak. Cu(II), Co(II), dan ARS
digunakan untuk membentuk kompleks berwarna dengan histamin. Kaedah yang telah dibangunkan digunakan untuk mengesan histamin
secara kualitatif
dan kuantitatif. Serapan kompleks Cu(II) dan Co(II) diukur pada panjang
gelombang maksimum masing-masing 505.5 dan 567 nm. Pengoptimuman parameter
analisis seperti kepekatan logam, kepekatan ARS, pH
larutan sampel, dan masa optimum bagi pembentukan kompleks telah dilakukan.
Keputusan eksperimen menunjukkan bahawa kepekatan optimum Cu(II) ialah 50 ppm,
75 ppm ARS, pH 6 larutan sampel, dan masa optimum 15 minit, manakala kepekatan
optimum Co(II) ialah 125 ppm, ARS ialah 75 dan 50
ppm, pH larutan sampel 5 dan 10 minit masa optimum. Pengesahan kaedah
menunjukkan bahawa pekali variasi (CV), had pengesanan (LOD) (S/N = 3) dan had
kuantititatif (LOQ = 10 S/N) Cu(II) masing-masing adalah 0.65%, 8.94 ppm dan 29.82 ppm dengan sensitiviti 0.0054 ppm dan
kelinearan 0.9959. Ketepatan penentuan histamin melalui kompleks
Cu-ARS-histamin pada kepekatan 50, 100, dan 150 ppm ialah 105.7% (RSD = 0.777%,
n = 3), 105.06% (RSD = 0.606%, n = 3), dan 94.12% (RSD
= 0.767%, n = 3), sementara itu,CV, LOD, dan LOQ Co(II) masing-masing adalah
0.28%; 2.58 ppm dan 8.6 ppm dengan kepekaan 0.0006 ppm dan kelinearan 0.9965.
Ketepatan penentuan histamin melalui kompleks Co-ARS-histamin pada kepekatan
50, 75, dan 125 ppm masing-masing adalah 98.33%,
95.83%, dan 93.88%. Kaedah yang dicadangkan berjaya digunakan untuk menentukan
histamin dalam sampel ikan dengan pengembalian kuantitatif untuk kompleks
Cu(II) (99.23%) dan kompleks Co(II) (102.62%).
Kata kunci: histamin, logam, Cu(II), Co(II), alizarin merah S, spektrofotometri
ultralembayung-nampak
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