An optimized SPE-UPLC-MS/MS method for simultaneous quantification of 11 tetracyclines in dairy products

Area of Science:

• Analytical Chemistry
• Food Science
• Pharmacology

Background:

• Rising antibiotic use in animal husbandry increases tetracycline (TC) residues in food.
• Current detection methods for TCs in dairy lack efficiency and multi-residue capability.
• Urgent need for rapid, precise, and cost-effective TC monitoring in dairy products.

Purpose of the Study:

• To develop and validate a streamlined method for simultaneous detection of multiple tetracyclines in dairy products.
• To ensure the method meets international maximum residue limits for food safety.

Main Methods:

• Integrated a three-step purification process (PRiME HLB cartridges) with UPLC-MS/MS.
• Utilized Na2EDTA-McIlvaine buffer for optimized extraction.
• Employed a BEH C18 column for rapid chromatographic separation.

Main Results:

• Achieved high recovery rates (83.11-107.61%) with low relative standard deviation (<5.43%).
• Enabled simultaneous detection of 11 TCs (parent compounds and metabolites) within 9 minutes.
• Demonstrated exceptional sensitivity with low limits of detection and quantification (0.02-0.83 μg/kg and 0.07-2.78 μg/kg).
• Validated intra-/inter-day precision (RSD 3.03-9.33%) in real milk and milk powder samples.

Conclusions:

• The developed method offers rapid sample preparation and simultaneous UPLC-MS/MS quantification of 11 TCs in dairy.
• High accuracy, sensitivity, and regulatory compliance make it vital for food safety monitoring.
• Addresses antibiotic residue risks and supports international trade harmonization.