Monitoring of melamine in milk and feed using ELISA and LCMS/MS screening methods

Suhaimi D.; Lily Suhaida M. S.; Ismail M.; Wan Syahidah H.

Monitoring of melamine in milk and feed using ELISA and LCMS/MS screening methods

2011

Suhaimi D. | Lily Suhaida M. S. | Ismail M. | Wan Syahidah H.

A monitoring program for melamine in milk and feed was conducted in response to global melamine alertness in the year 2008. Two screening methods were adopted i.e., a liquid chromatography triple quadrupole tandem mass spectrometry (LC-MS/MS) and enzyme-linkedimmunosorbent assay (ELISA). The liquid chromatography method developed by several international research centers was adapted. This method consisted of an initial extraction with 10%trichloroacetic acid (TCA) for milk samples or 60% methanol/water for feed samples, followed by a series of centrifugation, dilution and filtration steps. Melamine was analysed in the chromatographic program using a zwitterionic HILIC LC column. Electrospray ionisation in positive ion mode was used. The quantity of melaminepresent was determined with a calibration curve consisting of sample extracts from milk or feed fortified from 25 to 50 ppb that were taken through the extraction procedure. The ranges of recovery fromfortified raw milk samples (n=20) and feed samples (n=21) was 70–80% and 68%, respectively. The limit of detection was estimated at 10 ppb for both matrixes. Milk samples were found negative for melamine,however 4.5% of feed samples were found to contain the compound at concentrations between 1 to 5 ppm.

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