Determination of residues of aminoglycoside antibiotics in experiments
Determination of residues of aminoglycoside antibiotics in experiments
An aminoglycoside is a carbohydrate that contains one or more amino groups in its glycosidic structure. It is an antibiotic often used as a veterinary drug. Source: Food Safety Monitoring Technology (Chemical Industry Press)
Operation method
HPLC-MS/MS method
Materials and Instruments
Animal Tissue Move 1. Pre-treatment Weigh 2 g of sample in a 50 mL polypropylene centrifuge tube, add 3 mL of phosphate buffer (10 mmol/L KH2PO4 containing 0.4 mmol/LEDTA and 2% TCA), and homogenize (30-60 s). Plug firmly. Plug tightly and shake vigorously for l0 min. centrifuge at 4000 r/min for 10 min. transfer the supernatant to another centrifuge tube, add 10 mL of phosphate buffer/TAC to the residue, mix, and shake vigorously for l0 min. centrifuge and combine the supernatants. The combined supernatants were adjusted to pH 7.5-8.0 with 30% NaOH. centrifuged, and the fat was removed with an angular spoon if needed. SPE (BakerBondSPEWidePoreCB, 500 mg) column purification: the SPE column was loaded and drenched with 5 mL of MeOH and 5 mL of water. Samples were added at a flow rate of 1-3 mL/min, and the column was drenched with 4-5 mL of water and drained for 5 min. Aminoglycoside antibiotics were eluted with 3 mL of 0% acetic acid/methanol in a 1l5 mL glass centrifuge tube. Concentrate to approximately 0.1 mL with nitrogen at 40 °C and blow dry with nitrogen at room temperature. Add 0.4 mL of 5 mmol/L HFBA, mix and sonicate for 15 min, centrifuge for 10 min at 2500 r/min, transfer to another 0.6 mL polypropylene centrifuge tube and centrifuge for 10 min at 16,000 r/min. Carefully pipette about half of the supernatant into the autosampler bottle. 2. Instrument conditions Chromatographic column: reversed-phase C18 with an inner diameter of 2.1 mm and a length of 100 mm, 3.5 um particle size; Mobile phase: flow rate 0.15 mL/mm, initial 5% MeOH, 75% water, 20% 100 mmol/L HFBA. For more product details, please visit Aladdin Scientific website.
Phosphate buffer Acetic acid Methanol
SPE Columns Tubes