scholarly journals Detection of boldenone, its conjugates and androstadienedione, as well as five corticosteroids in bovine bile through a unique immunoaffinity column clean-up and two validated liquid chromatography–tandem mass spectrometry analyses

2014 ◽  
Vol 852 ◽  
pp. 137-145 ◽  
Author(s):  
L. Chiesa ◽  
M. Nobile ◽  
S. Panseri ◽  
C.A. Sgoifo Rossi ◽  
R. Pavlovic ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Immunoaffinity Column ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Bovine Bile

Determination of Ochratoxin A in Wine by Immunoaffinity Cleanup and Liquid Chromatography Tandem Mass Spectrometry

2008 ◽  
Vol 71 (5) ◽  
pp. 1038-1042 ◽  
Author(s):  
SHIGEKUNI NOBA ◽  
MASAYUKI OMOTE ◽  
YASUSHI KITAGAWA ◽  
NAOKI MOCHIZUKI
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ochratoxin A ◽  
Tandem Mass ◽  
Immunoaffinity Column ◽  
White Wines ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A simple and accurate method has been developed for determining ochratoxin A (OTA), using an immunoaffinity column for cleanup and liquid chromatography–tandem mass spectrometry for identification and quantification. Wine samples were diluted with a solution containing polyethylene glycol 8000 and sodium hydrogen carbonate, filtered through a glass microfiber filter, and cleaned up on an immunoaffinity column. OTA was then eluted with methanol–acetic acid (98:2) and analyzed by liquid chromatography–tandem mass spectrometry. The average recoveries of OTA from red and white wines were 95 and 96.7% (spiked OTA level was 0.05 ng/ml) and repeatabilities (relative standard deviation) were 3.8 and 2.4%, respectively. The detection limit was 0.0003 ng/ml based on the signal-to-noise ratio in wine of 3:1. Analysis of 74 samples of domestic and imported wines showed OTA levels ranging from <0.0003 to 0.82 ng/ml, with an incidence of contamination of 92.1% for red wines, and <0.0003 to 0.51 ng/ml, with an incidence of contamination of 77.8% for white wines. These detection rates were higher than those rates of past reports of OTA contamination in wine, due to the high sensitivity of this method. However, all samples analyzed in this study complied with European Union regulations. It is concluded that this method is a useful tool for the quality assurance of wine.

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