Method Validation for the Quantitative Analysis of Aflatoxins (B1, B2, G1, and G2) and Ochratoxin A in Processed Cereal-Based Foods by HPLC with Fluorescence Detection

2015 ◽  
Vol 98 (4) ◽  
pp. 939-945 ◽  
Author(s):  
Işil Gazioğlu ◽  
Ufuk Kolak
Keyword(s):  
Quantitative Analysis ◽  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Fluorescence Detection ◽  
Aflatoxin B1 ◽  
Hplc Analysis ◽  
Extraction Procedure ◽  
Immunoaffinity Column ◽  
Rp Hplc

Abstract Modified AOAC 991.31 and AOAC 2000.03 methods for the simultaneous determination of total aflatoxins (AFs), aflatoxin B1, and ochratoxin A (OTA) in processed cereal-based foods by RP-HPLC coupled with fluorescence detection were validated. A KOBRA® Cell derivatization system was used to analyze total AFs. One of the modifications was the extraction procedure of mycotoxins. Both AFs and OTA were extracted with methanol–water (75 + 25, v/v) and purified with an immunoaffinity column before HPLC analysis. The modified methods were validated by measuring the specificity, selectivity, linearity, sensitivity, accuracy, repeatability, reproducibility, recovery, LOD, and LOQ parameters. The validated methods were successfully applied for the simultaneous determination of mycotoxins in 81 processed cereal-based foods purchased in Turkey. These rapid, sensitive, simple, and validated methods are suitable for the simultaneous determination of AFs and OTA in the processed cereal-based foods.

scholarly journals Simultaneous Determination of Aflatoxins, Ochratoxin A, and Zearalenone in Grains by New Immunoaffinity Column/Liquid Chromatography

2004 ◽  
Vol 87 (2) ◽  
pp. 411-416 ◽  
Author(s):  
Roswitha Göbel ◽  
Klaus Lusky
Keyword(s):  
Column Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Fluorescence Detection ◽  
Trifluoroacetic Acid ◽  
Detection Limits ◽  
Immunoaffinity Column ◽  
Recovery Rates

Abstract The simultaneous determination of mycotoxins was performed in 3 steps: extraction, cleanup, and detection. For extraction, a mixture of acetonitrile–water (60 + 40, v/v) was proved appropriate. For cleanup, a new Afla-Ochra-Zea immunoaffinity column was used. After derivatization with trifluoroacetic acid, the mycotoxins aflatoxins, ochratoxin A (OTA), and zearalenone (ZEA) were determined simultaneously by liquid chromatography with fluorescence detection. The detection limits in different matrixes after cleanup with the new immunoaffinity column were very low: aflatoxins, 0.002–0.7 μg/kg; OTA, 0.07–0.25 μg/kg; ZEA, 1–3 μg/kg. The limits of determination were: aflatoxins, 0.25 μg/kg; OTA, 0.5 μg/kg; ZEA, 5 μg/kg. The recovery rates for aflatoxins, OTA, and ZEA for rye and rice were between 86 and 93% when a 0.5 g sample matter per immunoaffinity column was used.

scholarly journals Simultaneous Determination of Twenty Mycotoxins in the Korean Soybean Paste Doenjang by LC-MS/MS with Immunoaffinity Cleanup

Toxins ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 594 ◽  
Author(s):  
So Young Woo ◽  
So Young Ryu ◽  
Fei Tian ◽  
Sang Yoo Lee ◽  
Su Been Park ◽  
...  
Keyword(s):  
Measurement Uncertainty ◽  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Matrix Effect ◽  
Contamination Level ◽  
Immunoaffinity Column ◽  
Good Linearity ◽  
Soybean Paste ◽  
Contamination Levels

Doenjang, a Korean fermented soybean paste, is vulnerable to contamination by mycotoxins because it is directly exposed to environmental microbiota during fermentation. A method that simultaneously determines 20 mycotoxins in doenjang, including aflatoxins (AFs), ochratoxin A (OTA), zearalenone (ZEN), and fumonisins (FBs) with an immunoaffinity column cleanup was optimized and validated in doenjang using LC-MS/MS. The method showed good performance in the analysis of 20 mycotoxins in doenjang with good linearity (R2 > 0.999), intra- and inter-day precision (<16%), recovery (72–112%), matrix effect (87–104%), and measurement uncertainty (<42%). The validated method was applied to investigate mycotoxin contamination levels in commercial and homemade doenjang. The mycotoxins that frequently contaminated doenjang were AFs, OTA, ZEN, and FBs and the average contamination level and number of co-occurring mycotoxins in homemade doenjang were higher than those in commercially produced doenjang.

Determination of Ochratoxin A in Capsicum spp. (Paprika and Chili) by Immunoaffinity Column Cleanup and Liquid Chromatography: Collaborative Study

2014 ◽  
Vol 97 (3) ◽  
pp. 876-883 ◽  
Author(s):  
Zoltan Kunsagi ◽  
Joerg Stroka ◽  
E Abilleira ◽  
P Bastijns ◽  
M Berger ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Collaborative Study ◽  
Immunoaffinity Column ◽  
Fluorescence Detector ◽  
International Union ◽  
Eu Member States ◽  
Rp Hplc ◽  
Official Control ◽  
Capsicum Spp

Abstract A method validation study for the determination of ochratoxin A in Capsicum spp. (paprika and chili) was conducted according to the International Union of Pure and Applied Chemistry harmonized protocol. The method is based on the extraction of samples with aqueous methanol, followed by an immunoaffinity column cleanup. The determination is carried out by RP-HPLC coupled with a fluorescence detector. The study involved 21 participants representing a cross-section of research, private, and official control laboratories from 14 European Union (EU) Member States and Singapore. Mean recoveries reported ranged from 83.7 to 87.5%. The RSD for repeatability (RSDr) ranged from 1.7 to 14.3%. The RSD for reproducibility (RSDR) ranged from 9.1 to 27.5%, reflecting HorRat values from 0.4 to 1.3 according to the Horwitz function modified by Thompson. The correction for recovery of results from naturally contaminated samples further improved the reproducibility of the method. The method showed acceptable within-laboratory and between-laboratory precision for each matrix, and it conforms to requirements set by current EU legislation.

Sign in / Sign up

Export Citation Format

Share Document