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Wang G.,Chongqing Engineering Technology Research Center for Import and Export Food Safety | Zhao J.,Centers for Disease Control and Prevention | Peng T.,Chinese Academy of Inspection and Quarantine | Chen D.,Chinese Academy of Inspection and Quarantine | And 3 more authors.
Journal of Separation Science | Year: 2013

Matrix effects in determination of three β-receptor agonists including salbutamol (SAL), clenbuterol, and terbutaline in animal-derived foodstuffs were studied by ultra-performance LC-MS/MS with cleanup of immunoaffinity SPE column (IAC). Some animal tissue samples including pig liver, swine muscle, and fish muscle were hydrolyzed by the mixed enzyme solution or HCl solution, and the cleanup efficiencies with SAL IAC, MCX SPE column, and C18-SCX tandem columns were examined and compared by using spiked experiments. The results showed that the matrix effects in the determination of SAL and terbutaline can be eliminated with SAL IAC cleanup, and the average recoveries of SAL were 77.4∼81.5%, 79.0∼80.3%, and 85.0∼87.2% in pig liver, swine muscle, and fish muscle, respectively. The decision limit (ccα) and detection capability (ccβ) for SAL in pig liver were 0.02 and 0.05 μg/kg, respectively. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Xie J.,University of South China | Peng T.,Chinese Academy of Inspection and Quarantine | Chen D.-D.,Chinese Academy of Inspection and Quarantine | Zhang Q.-J.,University of South China | And 6 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2013

A high performance liquid chromatography method with visible detection (HPLC-VIS) for the determination of malachite green (MG), crystal violet (CV), leucomalachite green (LMG), and leucocrystal violet (LCV) in fish has been developed after clean-up through an immunoaffinity column (IAC). Residues were simultaneously extracted from fish muscle with acetonitrile and ammonium acetate buffer. The leuco-forms, LMG and LCV, were oxidized quantitatively to the chromic CV and MG by reaction with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone. Extracts were then purified on an IAC which prepared by immobilizing the anti-MG-CV antibodies by the sol-gel method. Finally, the eluents were analyzed by HPLC-VIS. The limits of detection were 0.15, 0.1, 0.18 and 0.14. ng/g for MG, CV, LMG and LCV, respectively. The average recoveries in samples fortified with MG, CV, LMG and LCV over the range 0.5-10. ng/g were from 71.6% to 96.8% with RSDs of 5.1-12.3% (n=6). This novel method was confirmed by liquid chromatography-tandem mass spectrometry with electrospray interface in positive mode using multiple reaction monitoring. © 2012 Elsevier B.V.

Li Y.,Chongqing University | Li Y.,Chongqing Engineering Research Center for Import and Export Food Safety | Chen Y.,China Agricultural University | Li Z.,Chongqing University | And 8 more authors.
Journal of Chromatographic Science | Year: 2012

This paper describes the preparation of a novel mixed-bed immunoaffinity chromatography (IAC) column by coupling four monoclonal antibodies against different sulfonamides (SAs) to Sepharose 4B. The IAC column can be used to simultaneously extract and purify 16 SAs in pork muscle. The dynamic column capacities for all SAs in mixed standard solution were between 312 and 479 ng/mL gel. After simple extraction and IAC cleanup, the sample solution can be directly injected for liquid chromatography-ultraviolet analysis. The recoveries of SAs from spiked samples at levels of 25, 50 and 100 g/kg ranged from 83.3 to 103.1 with variation coefficient less than 8.6. The comparison of IAC with liquidliquid extraction and solid phase extraction indicated that IAC has better purification effect and needs less organic solution than conventional methods, thus it would be an ideal method for selective purification of SAs in pork muscle. © 2012 The Author.

Zhang Q.-J.,University of South China | Peng T.,Chinese Academy of Inspection and Quarantine | Chen D.-D.,Chinese Academy of Inspection and Quarantine | Xie J.,University of South China | And 3 more authors.
Journal of AOAC International | Year: 2013

A method based on HPLC with UV detection was developed for the quantitative determination of chloramphenicol (CAP) residues in aquatic products. The samples were extracted with ethyl acetate-ammonium hydroxide (98 + 2, v/v), followed by a cleanup step using an immunoaffinity column. The analytes were determined by HPLC-UV. Optimal conditions for the extraction and cleanup procedures are described. The linear regression equation was y = 91.47× - 8.60 with R2 = 0.9998 (y = peak area and × = CAP concentration) and showed a good reproducibility. The LOQ was 0.25 μg/kg for determining CAP spiked in the aquatic products. The mean recoveries of CAP from fish and shrimp samples fortified at 0.25-1.0 μg/kg were 88.7-93.1 and 92.0-97.3%, respectively; the repeatability RSDs were less than 8.1%. It was concluded that the method is simple, highly sensitive, and low cost for quantitatively measuring CAP residues in aquatic products. Analyte identification was confirmed by HPLC/MS/MS analysis.

Zhao X.-T.,Shanxi University | Lin Q.-B.,Shanxi University | Song H.,Shanxi Border Inspection and Quarantine Bureau | Pan Y.-L.,Shanxi Border Inspection and Quarantine Bureau | Wang X.,Clover Technology Group Inc.
Journal of Agricultural and Food Chemistry | Year: 2011

A highly selective and sensitive method was developed for the simultaneous determination of 12 sulfonamides in beef and milk by immunoaffinity chromatography purification coupled to ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The MS/MS conditions, UPLC mobile phase, injection solution, sample purification process, and matrix effect were studied to optimize the operating conditions. The limits of detection (LODs) of the instrument for the studied sulfonamides ranged from 0.4 to 2.0 μg L -1, being 1.6-8.0 μg kg -1 for beef and 1.8-6.4 μg kg -1 for milk. The standard solution was diluted with blank beef or milk matrix for the construction of calibration curves, which had a linear range from 10 to 200 μg kg -1 and regression coefficients higher than 0.990 (n = 10) for all the studied sulfonamides. Samples spiked at 10, 20, and 100 μg kg -1 showed recoveries above 70% and relative standard deviations below 10%. © 2011 American Chemical Society.

Wang G.,Chongqing University | Li Y.,Chongqing University | Li X.,Chongqing Entry Exit Inspection and Quarantine Bureau | Wang X.,Clover Technology Group Inc. | And 4 more authors.
Journal of Chromatographic Science | Year: 2011

A rapid, simple, and reliable determination method for salbutamol in pork was developed with immunoaffinity column (IAC) extraction followed by HPLC analysis. The salbutamol immunoaffinity column was prepared by coupling CNBr-activated Sepharose-4B with the anti-salbutamol polyclonal antibody which was purified by caprylic acid-ammonium sulfate. The coupling rate of the antibody and Sepharose-4B was 98.6%, and the dynamic column capacity of IAC was 400 ng/mL gel. The average recoveries of salbutamol from spiked pork samples at levels of 2, 10, 20, and 50 ng/g ranged from 83.3% to 92.2%, with the relative standard deviations of 2.8-7.0% (n = 5), and the limits of detection and qualification were 0.25 ng/g and 0.5 ng/g, respectively.

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