Development and Validation of an UPLC-ESI-MS/MS Analytical Method for the Determination of Streptomycin and Dihydrostreptomycin Residues in Honey
Syed Amir Ashraf1
and Z. R. Azaz Ahmad Azad21Department of Food Technology, Faculty of Engineering, JJT University, Jhunjhunu, Rajasthan, India.
2Department of Food Technology, FEIS, Hamdard University, New Delhi, India.
Corresponding Author E-mail: zrazad.jamia@gmail.com
Abstract: The aim of present study was to develop and validate a rapid, precise, simple and sensitive method for the detection and quantification of streptomycin (STR) and dihydrostreptomycin (Di-STR) residues in honey using ultra performance liquid chromatography (UPLC) with electron spray ionization (ESI) tandem mass spectrometry. Separation of both the analytes were carried out by using BEH Hillic column 1.7 μm X 2.1 mm X 100 mm (Waters) and triple quadruple mass spectrometer in positive ESI mode. Two characteristics transitions of both the analytes were measured in multiple reaction monitoring mode. The method involved sample preparation in 2% acetic acid in water and acetonitrile followed by solid phase extraction and quantification by UPLC-MS/MS. The developed method was validated in accordance with European Commission Decision 2002/657/EC. The validation parameters were established for STR and Di-STR as CCα (11.68 and 11.27 µg kg-1 respectively), CCβ (13.36 and 12.55 µg kg-1 respectively) and average recovery was between 82-105%. The method presented showed adequate linearity with correlation coefficient above 0.994 for both analytes. Validation parameters were found to be satisfactory and within the European Commission Decision 2002/657/EC. Determination of STR and Di-STR confirms that, the validated method is suitable for routine analysis of commercially available honey samples. Finally, the validated method was applied for the determination of STR and Di-STR in 21 honey samples obtained from the local markets of New Delhi and Gurgaon, India.
Keywords: Antibiotic Residues; Honey; Method Validation;Streptomycin; UPLC-MS Back to TOC