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A validated dispersive liquid-liquid microextraction method for extraction of ochratoxin A from raisin samples
Rouhollah Karami-Osboo1, Ramin Miri1, Katayoun Javidnia1
1Medicinal and Natural Products Chemistry Research Centre, Shiraz University of Medical Sciences, Shiraz, Iran.
A new dispersive liquid-liquid microextraction (DLLME) method efficiently extracts Ochratoxin A (OTA) from raisins. This cost-effective technique offers high recovery and precision, with contamination levels below legal limits.
Area of Science:
- Analytical Chemistry
- Food Safety
Background:
- Ochratoxin A (OTA) is a mycotoxin found in various food products, including raisins.
- Accurate quantification of OTA is crucial for ensuring food safety and compliance with regulatory limits.
Purpose of the Study:
- To develop and validate a dispersive liquid-liquid microextraction (DLLME) method for the quantitative analysis of Ochratoxin A (OTA) in raisin samples.
- To optimize DLLME parameters for efficient OTA extraction and compare the method with a standard immunoaffinity column chromatography (IAC) technique.
Main Methods:
- Dispersive liquid-liquid microextraction (DLLME) was employed for OTA extraction from raisin samples.
- Optimization of DLLME parameters including extractant type/volume, centrifuging/sonication time, and deionized water volume.
- Analysis of OTA using optimized DLLME followed by comparison with immunoaffinity Column Chromatography (IAC) for validation.
Main Results:
- Optimized DLLME achieved recovery rates between 68.6% and 85.2%.
- High precision was observed with relative standard deviation (RSD%) below 15% for inner and intra-day variability.
- The method demonstrated linearity from 0.5 to 30 μg/L, with LOD of 0.7 μg/kg and LOQ of 2.0 μg/kg.
- Real raisin samples showed a mean OTA contamination of 0.88 μg/kg, below the European legal limit.
Conclusions:
- The developed DLLME method is a cost-effective, rapid, and simple technique for OTA quantification in raisins.
- The method offers low organic solvent consumption and high efficiency, making it suitable for routine analysis.
- The DLLME method provides reliable results comparable to IAC, ensuring food safety compliance.
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