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Quantitative Determination of 21 β-Agonists in Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
ZHANG Lijia, HU Xue, MO Nan, BAI Yanmei, ZHANG Yue, LIU Lijun, LI Cuizhi
Journal of Dairy Science and Technology    2020, 43 (3): 17-22.   DOI: 10.15922/j.cnki.jdst.2020.03.004
Abstract142)   HTML1)    PDF (2011KB)(116)       Save
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous quantitative determination of 21 β-agonists in milk. The samples were hydrolyzed and cleaned up a solid-phase extraction column. The analytes were separated by UPLC with an Acquity UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm) using a gradient mobile phase consisting of 0.1% formic acid aqueous solution and methanol (10 : 90, V/V). Identification and quantification were achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) under the positive ion mode The limit of quantitation of all β-agonists was 0.05 μg/kg. The average recovery varied from 61.0% to 124.3% at spiked concentration levels of 0.05, 0.10 and 0.50 μg/kg with relative standard deviations (RSDs) of 2.39%–10.66%. Our results demonstrate that the method is stable, accurate and sensitive, and can be used for the determination of the 21 β-agonists residues in milk.
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Quantitative Determination of Salicylic Acid in Milk and Dairy Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
HU Xue, ZHANG Yue, ZHANG Lijia, MO Nan, DUAN Guoxia, LIU Lijun, LI Cuizhi
Journal of Dairy Science and Technology    2019, 42 (3): 29-32.   DOI: 10.15922/j.cnki.jdst.2019.03.006
Abstract162)   HTML0)    PDF (1631KB)(151)       Save
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the quantitative determination of salicylic acid in milk and dairy products was developed. The sample was extracted with 1% acidified acetonitrile, and then the extract was purified by solid-phase extraction (SPE) with an HLB cartridge. The separation was performed on an Acquity UPLC BEH C18 chromatographic column (50 mm × 2.1 mm, 1.7 μm)with gradient elution using 0.1% aqueous formic acid-acetonitrile as the mobile phase. The target compound was monitored under the negative ion mode with an electrospray ionization (ESI) source and quantified by external standard method. The results demonstrated that the linear range of the proposed method was from 0.5 to 50.0 ng/mL with a correlation coefficient (R2) > 0.999. The average recovery of salicylic acid in different matrixes spiked at low, medium and high levels varied from 68.3% to 111.7%, and the relative standard deviations (RSDs) of precision were between 3.3% and 15.2%. The limits of detection (LODs) were 5.0 and 10.0 μg/kg in milk and milk powder, respectively. This method can meet the requirements for the determination of different salicylic acid levels in milk and dairy products.
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