A Novel and Sensitive LC-MS/MS Method for the Quantitation of Ceftiofur in Pharmaceutical Preparations and Milk Samples

Author(s): Serkan Levent, Saniye Özcan, Aysun Geven, Nafiz Öncü Can*

Journal Name: Combinatorial Chemistry & High Throughput Screening
Accelerated Technologies for Biotechnology, Bioassays, Medicinal Chemistry and Natural Products Research

Volume 24 , Issue 3 , 2021

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Introduction: In the present study, a sensitive and selective liquid chromatographytandem mass spectrometry (LC-MS/MS) method was described for the determination of ceftiofur (CEF) in cow milk and pharmaceutical preparations. CEF is an antibiotic compound, which is commonly used in the treatment of animal diseases such as respiratory system, soft tissue, and foot infections, as well as postpartum acute puerperal metritis. One of the critical features of CEF is its prescription while breastfeeding cows; in accordance, its quantitative estimation is essential to assess its residual amounts.

Methods: In the method reported herein, after simple protein precipitation using acetonitrile, the pre-treated samples were introduced into an LC-MS/MS instrument equipped with a Chromolith® High-Resolution RP-18 series HPLC column (100 mm × 4.6 mm from Merck KGaA, Germany). Electrospray ionization was employed as the ionization source in the triple-quadrupole tandem mass spectrometer.

Results: For the calibration method using solvent-based standards, LOQ was 3.038 ng/mL, 12.15 ng/mL, and LOD was 1.215 ng/mL and 6.076 ng/mL for ESI+ and ESI- modes, respectively. On the other hand, for the method of matrix-matched standards, LOQ was 1.701 ng/mL, 10.13 ng/mL, and LOD was 0.486 ng/mL and 5.929 ng/mL for ESI+ and ESI- modes, respectively as obtained from signal to noise ratio.

Conclusion: Applicability of both positive and negative ion modes was tested, and the analyte was detected via multiple reaction monitoring. The distorting effects of the milk matrix on the MS ionization and quantitation of CEF were overcome by using matrix-matched calibration for the first time.

Keywords: Ceftiofur, solvent-based calibration, LC-MS/MS, matrix-matched calibration, milk analysis, monolithic silica column.

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Article Details

Year: 2021
Published on: 18 February, 2021
Page: [386 - 399]
Pages: 14
DOI: 10.2174/1386207323999201110192558
Price: $65

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