Analysis of Deoxynivalenol, Zearalenone, T-2, and HT-2 Toxins in Animal Feed by LC/MS/MS-A Critical Comparison of Immunoaffinity Column Cleanup with No Cleanup

Senyuva, Hamide Z.
Gilbert, John
Turkoz, Gozde
Leeman, David
Donnelly, Carol
A comparison has been made of an LC/MS/MS method using direct analysis of acetonitrile extracts of feed and cereal samples and a method using acetonitrile extraction and subsequent immunoaffinity column (IAC) cleanup. Naturally contaminated samples containing one or more of deoxynivalenol, zearalenone, T-2, and HT-2 toxins were analyzed together with test materials containing known toxin levels. LC/MS/MS ion ratios and peak profiles, repeatability, and LOQs were used as the basis for comparing the two approaches. The method without cleanup had poorer performance than the method with IAC cleanup in terms of identification based on ion ratios compared to standards. Without cleanup, there was more evidence of background interference, and monitored ions were invariably seen against a noisy background. Nevertheless, quantification of samples analyzed without cleanup gave reasonable agreement with the levels found in the same samples that had received IAC cleanup. Repeatability was poorer with no cleanup, and LOQ values were higher for HT-2 and 1-2 toxins, but there was no evidence of any adverse effects on MS performance with repeated injections of crude extracts. Overall, it was concluded that LC/MS/MS analysis of samples with no cleanup is adequate for screening, but for definitive measurements (e.g., for food regulatory control purposes) IAC cleanup remains essential.


Immunoaffinity Column Cleanup with Liquid Chromatography Using Postcolumn Bromination for the Determination of Aflatoxins in Black and White Sesame Seed: Single-Laboratory Validation
Liu, Guihua; Zhu, Zhou; Cheng, Jinquan; Senyuva, Hamide Z. (Oxford University Press (OUP), 2012-01-01)
A single-laboratory validation was conducted to establish the effectiveness of an immunoaffinity column cleanup procedure followed by LC with fluorescence detection for the determination of aflatoxins B-1, B-2, G(1), and G(2) in sesame seeds. The sample is homogenized with 50% water (w/w) to form a slurry, then the test portion is extracted with methanol-water (60 + 40, v/v) using a high-speed blender. The sample extract is filtered, diluted with 15% Tween 20 in phosphate-buffered saline solution, and appli...
Determination of Ochratoxin A in Black and White Pepper, Nutmeg, Spice Mix, Cocoa, and Drinking Chocolate by High-Performance Liquid Chromatography Coupled with Fluorescence Detection: Collaborative Study
Cubero-Leon, Elena; Bouten, Katrien; Senyuva, Haviide; Stroka, Joerg (Oxford University Press (OUP), 2017-09-01)
A method validation study for the determination of ochratoxin A in black and white pepper (Piper spp.), nutmeg (Myristica fragrans), spice mix (blend of ginger, turmeric, pepper, nutmeg, and chili), cocoa powder, and drinking chocolate was conducted according to the International Harmonized Protocol of the International Union of Pure and Applied Chemistry. The method is based on the extraction of samples with aqueous methanol, followed by a cleanup of the extract with an immunoaffinity column. The determina...
Determination of Arsenobetaine in Fish Tissue by Species Specific Isotope Dilution LC-LTQ-Orbitrap-MS and Standard Addition LC-ICPMS
Yang, Lu; Ding, Jianfu; Maxwell, Paulette; McCooeye, Margaret; Windust, Anthony; Ouerdane, Laurent; Bakirdere, Sezgin; Willie, Scott; Mester, Zoltan (American Chemical Society (ACS), 2011-05-01)
An accurate and precise method for the determination of arsenobetaine (AsB, (CH(3))(3)(+)AsCH(2)COO(-)) in fish samples using exact matching species specific isotope dilution (ID) liquid chromatography LTQ:Orbitrap mass spectrometry (LC-LTQ-Orbitrap-MS) and standard addition LC inductively coupled plasma mass spectrometry (LC-ICPMS) is described. Samples were extracted by sonication for 30 min with high purity deionized water. An in-house synthesized (13)C enriched AsB spike was used for species specific ID...
Rapid LC and LC/MS for routine analysis of mycotoxins in foods
Senyuva, H.; Gilbert, J.; Özcan Kabasakal, Süreyya; Gurel, N. (Wageningen Academic Publishers, 2008-08-01)
Affinity column clean-up of food samples for mycotoxin analysis produces extracts which are free of co-extractives and therefore require little chromatography for separation and quantification of the target analytes. Using such clean extracts, we report rapid chromatographic methods for aflatoxins B(1), B(2), G(1) and G(2), aflatoxin M(1), ochratoxin A, zearalenone and fumonisins. Using short columns with small particle size packing, HPLC conditions have been developed reducing analysis time typically by 75...
CABBAR, C; DOGU, G; Doğu, Timur; MCCOY, BJ; SMITH, JM (American Chemical Society (ACS), 1994-07-01)
The single-pellet moment technique was shown to be a powerful method for investigating the diffusion and adsorption of volatile hydrocarbons in the soil. The technique was used to evaluate effective diffusivities, adsorption equilibrium, and rate constants of chlorinated hydrocarbons (monochloroethane, 1,2-dichloroethane, 1,1,1-trichloroethane, and 1,1,2-trichloroethane). Results obtained in a dry system showed that adsorption rate constants of all these hydrocarbons on the soil pellet used are of the same ...
Citation Formats
H. Z. Senyuva, J. Gilbert, G. Turkoz, D. Leeman, and C. Donnelly, “Analysis of Deoxynivalenol, Zearalenone, T-2, and HT-2 Toxins in Animal Feed by LC/MS/MS-A Critical Comparison of Immunoaffinity Column Cleanup with No Cleanup,” JOURNAL OF AOAC INTERNATIONAL, pp. 1701–1708, 2012, Accessed: 00, 2020. [Online]. Available: