| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1242050 | Talanta | 2015 | 6 Pages |
•Three procedures for melamine extraction from powdered milk were evaluated.•Extraction based on melamine precipitation using trichloroacetic acid was suitable.•The melamine concentration in powdered milk was determined using ESI–MS/MS.•The nature of melamine in the extract was characterized using infrared spectroscopy and microscopy.
A combination of a simple pretreatment for melamine extraction and direct analysis in electrospray ionization tandem mass spectrometry (ESI–MS/MS) is proposed. Three pretreatments were evaluated. The first was based on suppressing interference using acetonitrile. The second used sulphuric acid and trichloroacetic acid to suppress interference and for melamine extraction, respectively. The third used sulphuric acid to suppress milk interference, trichloroacetic acid for melamine precipitation, and ethyl acetate for melamine extraction. However, only the last pretreatment suppressed milk interference in melamine detection and a good linearity (R2=0.99) was obtained. The presence of MS/MS 85 on melamine fragmentation spectrum showed the selectivity of this method. The limit of detection and limit of quantification were 0.269 µg L−1 and 0.897 µg L−1, respectively. The recoveries and relative standard deviation (RDS) of method were lower than 114% and 7.86%, respectively. Further, the research was extended to elucidate the nature of the melamine in the extract through infrared spectroscopy and microscopy analyses. The precipitate was characterized as melaminium bis(trichloroacetate) dihydrate, which is generated through hydrogen bound formation in an interaction between melamine and trichloroacetic acid. Therefore, a simple, fast, and easy method for melamine extraction and direct ESI–MS/MS analysis was developed.
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