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Blackburn M.A.,Covance | Kapron J.,Thermo Fisher Scientific | Mackie J.,R Biopharm Rhone Ltd | Firth J.,Covance | And 2 more authors.
Bioanalysis | Year: 2011

Background: The determination of pharmacokinetic parameters requires accurate and reliable bioanalytical methods. Even using highly selective MS/MS, interferences can occur. This paper describes the source of some of these interferences with an example discussed involving the problem of a ketamine interference in a plasma assay. Results: The introduction of field asymmetric waveform ion mobility spectrometry (FAIMS) removed the interference, enhanced signal-to-background and met GLP acceptance criteria. Relative to the non-FAIMS method, assay calibration characteristics were improved. The FAIMS source gave optimal performance following the introduction of a split in order to reduce the inlet flow to approximately 0.4 ml/min. Conclusion: The introduction of ion-mobility separation into a bioanalytical LC-MS/MS method can remove unexpected isobaric interferences without the need to redevelop the chromatography. © 2011 Future Science Ltd. Source


Tanaka H.,Japan National Institute of Health Sciences | Takino M.,Agilent Technologies | Sugita-Konishi Y.,Japan National Institute of Health Sciences | Tanaka T.,Kobe Institute of Health | And 3 more authors.
Rapid Communications in Mass Spectrometry | Year: 2010

A method for the simultaneous quantitative determination of deoxynivalenol (DON), T-2 toxin (T-2), HT-2 toxin (HT-2) and zearalenone (ZEN) in wheat and biscuit by liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) coupled with immunoaffinity extraction is described. A clean-up was carried out using a DZT MS-PREP® immunoaffinity column (IAC), and the effect of the sample dilution rate and sample loading was investigated. Furthermore, the effects of ion suppression of a multifunctional column (MFC) and the IAC in the clean-up were compared. The results with the DZT MS-PREP® IAC showed that it is possible to make the sample dilution rate low, and indicated a higher solvent-tolerance than usual with an IAC. Sample loading was optimized at 0.25 g. Ion suppression was lowered by purification of the toxins using the DZT MS-PREP® IAC. Recoveries of each mycotoxin from wheat and biscuit samples spiked at two levels ranged from 78 to 109%. The limits of detection in wheat and biscuit was in the range of 0.03-0.33 ng g-1. From these studies, it is suggested that use of an IAC is effective in the clean-up of each mycotoxin, and, when combined with LC/ESI-MS/MS, it is good for the determination of mycotoxins in foodstuffs due to its rapidity and high sensitivity. © 2010 John Wiley & Sons, Ltd. Source


Marley E.,R Biopharm Rhone Ltd | Brown P.,R Biopharm Rhone Ltd | Mackie J.,R Biopharm Rhone Ltd | Donnelly C.,R Biopharm Rhone Ltd | And 3 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2015

A method is reported for the analysis of sterigmatocystin in various food and feed matrices using a commercial sterigmatocystin immunoaffinity column (IAC) for sample clean-up prior to HPLC analysis by UV with mass spectrometric detection (LC-MS/MS). Cereals (wheat, oats, rye, maize and rice), sunflower seeds and animal feed were spiked with sterigmatocystin at levels from 0.75 to 50 µg kg−1 to establish method performance. Using acetonitrile/water extraction followed by IAC clean-up, and analysis by HPLC with detection at 325 nm, recoveries ranged from 68% to 106%, with repeatability from 4.2% to 17.5%. The limit of quantification with UV detection in these matrices was 1.5 µg kg−1. For the analysis of beer and cheese the sample preparation prior to IAC clean-up was changed to accommodate the different properties of the matrix, prior to analysis by LC-MS/MS. For beer and cheese spiked at 5.0 µg kg−1 the recoveries were 94% and 104%, and precision (RSDs) were 1.9% and 2.9% respectively. The limits of quantification by LC-MS/MS in beer and cheese were 0.02  and 0.6 µg kg−1 respectively. The sterigmatocystin IAC was demonstrated to provide an efficient clean-up of various matrices to enable this mycotoxin to be determined by either HPLC with UV detection or LC-MS/MS. © 2015 Taylor & Francis. Source


Senyuva H.Z.,Middle East Technical University | Gilbert J.,Middle East Technical University | Turkoz G.,Turizm San. ve Tic. Ltd STI | Leeman D.,R Biopharm Rhone Ltd | Donnelly C.,R Biopharm Rhone Ltd
Journal of AOAC International | Year: 2012

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 T-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. Source


Rhemrev R.,R Biopharm Rhone Ltd | Pazdanska M.,R Biopharm Rhone Ltd | Marley E.,R Biopharm Rhone Ltd | Biselli S.,Eurofins | Staiger S.,Eurofins
Journal of AOAC International | Year: 2015

A novel reusable immunoaffinity cartridge containing monoclonal antibodies to aflatoxins coupled to a pressure resistant polymer has been developed. The cartridge is used in conjunction with a handling system inline to LC with fluorescence detection to provide fully automated aflatoxin analysis for routine monitoring of a variety of food matrixes. The handling system selects an immunoaffinity cartridge from a tray and automatically applies the sample extract. The cartridge is washed, then aflatoxins B1, B2, G1, and G2 are eluted and transferred inline to the LC system for quantitative analysis using fluorescence detection with postcolumn derivatization using a KOBRA® cell. Each immunoaffinity cartridge can be used up to 15 times without loss in performance, offering increased sample throughput and reduced costs compared to conventional manual sample preparation and cleanup. The system was validated in two independent laboratories using samples of peanuts and maize spiked at 2, 8, and 40 μg/kg total aflatoxins, and paprika, nutmeg, and dried figs spiked at 5, 20, and 100 μg/kg total aflatoxins. Recoveries exceeded 80% for both aflatoxin B1 and total aflatoxins. The between-day repeatability ranged from 2.1 to 9.6% for aflatoxin B1 for the six levels and five matrixes. Satisfactory Z-scores were obtained with this automated system when used for participation in proficiency testing (FAPAS®) for samples of chilli powder and hazelnut paste containing aflatoxins. Source

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