Simultaneous Determination of Aflatoxins and Ochratoxin A in Bee Pollen by Low-Temperature Fat Precipitation and Immunoaffinity Column Cleanup Coupled with LC-MS/MS

2013 ◽  
Vol 7 (3) ◽  
pp. 690-696 ◽  
Author(s):  
XiaoFeng Xue ◽  
Jonathan Nimal Selvaraj ◽  
Liuwei Zhao ◽  
Haimin Dong ◽  
Fengmao Liu ◽  
...  
Keyword(s):  
Low Temperature ◽  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Immunoaffinity Column ◽  
Bee Pollen

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.

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.

Determination of Ochratoxin A in Feed by Immunoaffinity Cleanup and Liquid Chromatography

2013 ◽  
Vol 96 (3) ◽  
pp. 599-602 ◽  
Author(s):  
Ping Ding ◽  
Ziyou Mi ◽  
Yali Hou ◽  
Yigang He ◽  
Jianhua Xie
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Ochratoxin A ◽  
Cyanogen Bromide ◽  
Polyclonal Antibodies ◽  
Immunoaffinity Column ◽  
Low Levels ◽  
Sepharose 4B ◽  
Feed Samples

Abstract A method using LC was developed for determination of ochratoxin A (OTA) in feeds. The extracted samples were cleaned up by an immunoaffinity column prepared by covalently coupling polyclonal antibodies against OTA to cyanogen bromide-activated Sepharose 4B. The eluates were determined by LC with fluorescence detection. Recoveries of OTA from fortified samples of 1–10 μg/kg levels ranged from 84.3 to 90.0%, with CVs of 3.3–7.8%. The detection limit was 0.045 μg/kg based on an S/N of 3:1. A total of 65 feed samples were screened for OTA with the proposed method. The results showed that only nine samples were contaminated with OTAs at low levels. The presented method was successfully applied to quantify OTAs in real feed samples.

Development and validation of an LC–MS/MS method for the simultaneous determination of citrinin and ochratoxin a in a variety of feed and foodstuffs

2018 ◽  
Vol 1580 ◽  
pp. 100-109 ◽  
Author(s):  
Celine Meerpoel ◽  
Arnau Vidal ◽  
José Diana di Mavungu ◽  
Bart Huybrechts ◽  
Emmanuel K. Tangni ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Ochratoxin A ◽  
Development And Validation

scholarly journals Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

2009 ◽  
Vol 61 (4) ◽  
pp. 639-644 ◽  
Author(s):  
Gorica Vukovic ◽  
Snezana Pavlovic ◽  
M.S. Ristic
Keyword(s):  
Sample Preparation ◽  
Phosphoric Acid ◽  
Ochratoxin A ◽  
Chromatographic Determination ◽  
Liquid Extraction ◽  
Immunoaffinity Column ◽  
Maize Flour ◽  
Liquid Liquid Extraction ◽  
Immunoaffinity Columns

In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns). The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec?ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf?finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2) for the first method of sample preparation and 101% (%RSD = 2.2) for the second method. Values of LOQ for OTA were 0.25 and 1.00 ?g/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

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