Thursday, September 18, 2008

Decent HPLC Assay Method for Melamine

(From FDA: Melamine found in baby formula made in China.)

I am really feel sorry for the innocent baby. Feel shame for the authority in SFDA in China. They are not doing any professional jobs.


Sample Pre-treatment:
Transfer an accurately weighted quantity (5 g) of Baby (Infant) formula or milk powder sample to 50-mL volumetric flask. Add some amount of grade MeOH and mix well, sonicate it 10 min. Bring to volume with MeoH. Filter through a membrane filter (0.22 um) before injection.


Standard Preparation:
Using an accurately weighted quantity (50 mg) of USP Melamine RS, prepare a solution in MeOH having a known concentration of about 1 mg/ml.

Column: C18 4.6×250mm,5um.
Buffer:10mM Citric Acid, 10mM 1-Heptanesulfonic acid. using 1M NaOH adjust pH to 3.0.
Mobile Phase: Buffer:MeCN=85:15.
Injection Volume: 10uL.
Flow rate: 1.0mL/min.
Column Temp: 30℃.
Detector Wavelength: 236nm or DAD.