Optimization and Validation of Dispersive Liquid-Liquid Microextraction for Simultaneous Determination of Aflatoxins B1, B2, G1, and G2 in Senna Leaves and Pods Using HPLC-FLD with Pre-Column Derivatization

Dispersive liquid-liquid microextraction (DLLME) was optimized for the simultaneous extraction of aflatoxins (AFB1, AFB2, AFG1, and AFG2) from powdered senna leaves and pods. Detection was performed using high-performance liquid chromatography with fluorescence detection (HPLC-FLD) and pre-column de...

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Bibliographic Details
Published in:Toxins 2023-04, Vol.15 (4), p.277
Main Authors: Maneeboon, Thanapoom, Chuaysrinule, Chananya, Mahakarnchanakul, Warapa
Format: Article
Language:English
Subjects:
Aflatoxin B1 - analysis
Aflatoxins
Aflatoxins - analysis
Agricultural commodities
Aqueous solutions
Carcinogens
Chloroform
Chromatography, High Pressure Liquid - methods
Control
Dispersion
Distilled water
DLLME
Efficiency
Extraction (Chemistry)
Herbal medicine
Herbs
High performance liquid chromatography
HPLC-FLD
Limit of Detection
Liquid chromatography
Liquid Phase Microextraction
medicinal herb
Methods
mycotoxin
Optimization
Physiological aspects
Regression coefficients
Senna
Solvents
Variance analysis
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Summary:Dispersive liquid-liquid microextraction (DLLME) was optimized for the simultaneous extraction of aflatoxins (AFB1, AFB2, AFG1, and AFG2) from powdered senna leaves and pods. Detection was performed using high-performance liquid chromatography with fluorescence detection (HPLC-FLD) and pre-column derivatization. The parameters affecting the DLLME extraction efficiency were evaluated. Chloroform (200 µL) was used as an extraction solvent, 500 µL of distilled water was used as a dispersive solvent, and the extraction was performed at pH 5.6 with no salt added. The optimized method was validated using leaves and pods according to the European Commission guidelines. The linear range for all aflatoxins was 2-50 µg/kg, with values for regression coefficients of determination exceeding 0.995. The recoveries of spiked senna leaves and pods were in the ranges of 91.77-108.71% and 83.50-102.73%, respectively. The RSD values for intra-day and inter-day precisions were in the ranges of 2.30-7.93% and 3.13-10.59%, respectively. The limits of detection and quantification varied in the ranges of 0.70-1.27 µg/kg and 2.13-3.84 µg/kg, respectively. The validated method was successfully applied for the quantification of aflatoxins in 60 real samples of dried senna leaves and pods.
ISSN:2072-6651
2072-6651
DOI:10.3390/toxins15040277