Melamine in dog food by GC/MS using a ZB-5MSplus (EIC)

GC Conditions

Column

Zebron ZB-5MSplus, GC Cap. Column 30 m x 0.25 mm x 0.25 µm, EA

Part No

7HG-G030-11

Phase Name

ZB-5MSplus

Injection

Splitless @ 280°C

Oven Program

75º C for 1 min to 320 ºC at 15 ºC/min hold for 4 min

Carrier Gas

Constant Flow Helium, 1.0 mL/min

Detection

Mass Selective (MSD) @ (320°C)

Detection Info

Sample Notes

Sample preparation: Combine 0.5 g of homogenized dog food with 10 mL of DEA/water/acetonitrile (1:4:5) in a 15 mL centrifuge tube. Sonicate for 30 min. Centrifuge at 5000 rpm for 10 min. Transfer 100 µL of supernatant to an autosampler vial and evaporate to dryness using nitrogen gas. Reconstitute with 100 µL of acetonitrile/pyridine (1:1) and then derivatize using 100 µL of BSTFA with 1% TCMS at 70 ºC for 45 min. Inject sample into the GC/MS. Dry dog food spiked with 100 µg/g melamine and related compounds. Sim mode: Cyanuric acid (345,330,346), Ammelide (344,329,345), Ammeline (328,343,329), Melamine (327,342,328), Benzoguanamine (316,331,332)