This is an Application Brief and does not contain a detailed Experimental section.
This application brief describes method to determine dexamethasone in pork.
The European Union (EU) considers dexamethasone residues a high priority in food animals as they are synergistic with illegal growth promoters, such as beta-agonists or anabolic steroids.
1. Add 5 g of the ground pork into 30 mL of 95:5 acetonitrile:water (v/v).
2. Shake for 20 minutes, homogenize, and shake for 10 minutes.
3. Centrifuge for 5 minutes.
4. Repeat extraction.
5. Combined both extractions and load onto Sep-Pak Vac 3 cc (500 mg), Florisil Cartridges and elute with 30 mL of 95% acetonitrile and bring up to 100 mL with acetonitrile.
6. Take out 20 mL of extract add 10 mL of hexane. Shake for 3 minutes and leave to stand.
7. Take acetonitrile layer and evaporate to dryness.
8. Reconstitute with 4 mL of 0.2 M sodium phosphate buffer (pH 5) to a final volume of 6 mL with water.
System: |
ACQUITY UPLC |
Column: |
ACQUITY UPLC BEH C18, 1.7 μm, 2.1 x 100 mm |
Flow rate: |
400 μL/min |
Mobile phase A: |
0.1% formic acid in water |
Mobile phase B: |
0.1% formic acid in acetonitrile |
Time (min) |
A% |
B% |
---|---|---|
0.00 |
70 |
30 |
3.00 |
10 |
90 |
3.10 |
70 |
30 |
4.00 |
70 |
30 |
MS System: |
Waters Quattro Premier |
Ionization mode: |
Positive electrospray (ESI+) Multiple reaction monitoring |
720002599, April 2008