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Development Of Purity Reference Materials Of Nitrofuran Metabolites And Matrix Reference Materials Of Melamine

Posted on:2012-12-23Degree:MasterType:Thesis
Country:ChinaCandidate:L LuFull Text:PDF
GTID:2131330335999482Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
3-amino-2-oxazolidinone and 3-amino-5-morpholinomethyl-2-oxazolidinone are prepared and certified as pure reference material. IR spectrum and LC-MS method are used to identify the structure of the material. High performance liquid chromatography-diode array detector (HPLC-DAD), gas chromatography-hydrogen flame ionization detector (GC-FID) and Differential scanning calorimeter (DSC) are optimized and established for the principal component value. Karl fischer method, inductively coupled plasma mass spectrometry(ICP-MS) and hermo gravimetric analyzer were used to determine moisture and inorganic impurities. Test results show that 3-amino-2-oxazolidinone and 3-amino-5-morpholinomethyl-2-oxazolidinone are homofeneous. It is found to be stable at least 7 months. The certified purity value of 3-amino -2-oxazolidinone is 99.50%, the expanded uncertainty is 0.86%(k=2); 3-amino-5-morpholinomethyl-2-oxazolidinone is 99.28%, the expanded uncertainty is 0.50% (k=2), respectively. High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) are optimized and established for the melamine value in milk powder. The purity and the expanded combined uncertainty are 3.564 mg/kg±0.152 (k=2) and 0.446 mg/kg±0.039 (k=2), respectively.
Keywords/Search Tags:3-amino -2-oxazolidinone (AOZ), reference material, purity, melamine, 3-amino-5-marpholinomethyl-2-oxazolidinone(AMOZ)
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