Measuring Ochratoxin A Concentrations in Coffee Beverages with Immunoaffinity Columns and Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry

2016 ◽  
Vol 99 (2) ◽  
pp. 469-474 ◽  
Author(s):  
Wen-Ling Chen ◽  
Chiung-Wen Chang ◽  
Chia-Yang Chen

Abstract This study developed and validated a method for measuring concentrations of ochratoxin A (OTA) in coffee beverages, not coffee beans. The new method involved extraction using immunoaffinity columns and ultra-performance LC (UPLC)-MS/MS using isotope-dilution techniques. The combination of a fused-core column and UPLC significantly shortened chromatographic time to 3 min compared to reported UPLC methods. The method was sensitive, with an LOD and LOQ of 0.52 and 1.73 pg/mL, respectively. Quantitative intraday (n = 4) and interday (n = 4) biases and RSD were both below 15%. The OTA levels in 40 samples of freshly brewed coffee from chain stores, 24 samples of canned ready-to-drink coffee, and 6 beverages made from instant coffee granules ranged from 1.60 to 93.2 pg/mL (90% positive), 6.00 to 131 pg/mL (100% positive), and 21.8 to 59.0 pg/mL (100% positive), respectively. Based on published tolerable daily intake, men and women in Taiwan should consume no more than 6.3 and 5.1 fifteen gram packages of instant coffee per day, respectively. Specific suggestions were not made for brewed coffee and canned coffee because of their large variation in OTA concentrations. This study should be more relevant to actual human exposure than those studying OTA in green, roasted, and ground coffee beans alone.

2014 ◽  
Vol 97 (5) ◽  
pp. 1384-1386 ◽  
Author(s):  
Kieu Thi Ngoc Nguyen ◽  
Dojin Ryu

Abstract A rapid, simple, and reliable method using ultra-performance LC/MS/MS (UPLC/MS/MS) was developed for determination of ochratoxin A (OTA) in processed cereal products. OTA was ultrasonically extracted from the sample with acetonitrile–water (80 + 20, v/v), and the extract was then injected into the UPLC/MS/MS system after filtration. The calibration curves had good linearity with coefficients of determination greater than 0.999. Recoveries of OTA were in the range of 90–104%. LOD and LOQ of OTA in samples were 0.6 and 2.0 ng/g, respectively, and no significant matrix effect was found. This method was applied to determine OTA in 25 oat-based cereal samples. OTA was detected in five samples (20%) in the range of 2.4 to 7.3 ng/g.


Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 188
Author(s):  
Agnieszka Zapaśnik ◽  
Marcin Bryła ◽  
Agnieszka Waśkiewicz ◽  
Edyta Ksieniewicz-Woźniak ◽  
Grażyna Podolska

The aim of this study was to estimate the contamination of grain coffee, roasted coffee, instant coffee, and cocoa purchased in local markets with ochratoxin A (OTA) and its isomerization product 2′R-ochratoxin A (2′R-OTA), and to assess risk of dietary exposure to the mycotoxins. OTA and 2′R-OTA content was determined using the HPLC chromatography with immunoaffinity columns dedicated to OTA. OTA levels found in all the tested samples were below the maximum limits specified in the European Commission Regulation EC 1881/2006. Average OTA concentrations calculated for positive samples of grain coffee/roasted coffee/instant coffee/cocoa were 0.94/0.79/3.00/0.95 µg/kg, with the concentration ranges: 0.57–1.97/0.44–2.29/0.40–5.15/0.48–1.97 µg/kg, respectively. Average 2′R-OTA concentrations calculated for positive samples of roasted coffee/instant coffee were 0.90/1.48 µg/kg, with concentration ranges: 0.40–1.26/1.00–2.12 µg/kg, respectively. In turn, diastereomer was not found in any of the tested cocoa samples. Daily intake of both mycotoxins with coffee/cocoa would be below the TDI value even if the consumed coffee/cocoa were contaminated with OTA/2′R-OTA at the highest levels found in this study. Up to now only a few papers on both OTA and 2′R-OTA in roasted food products are available in the literature, and this is the first study in Poland.


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