Melamine detected in milk and dairy products – melamine, melamine detected – Food Industry
Food Safety Implementation of the law strengthened Food enterprises For product quality testing, particularly Dairy , Dairy products, etc. Food And livestock Feed In Melamine Quantitative analysis, with more stringent requirements.
Dairy , Dairy food and livestock feed in the quantitative analysis of melamine can use high performance liquid chromatography and liquid chromatography-mass spectrometry (LC-MS/MS) or GC (GC-MS) are three main ways. Regardless of which method, sample preparation is the first and most crucial step. Sample pretreatment to protect the effective separation of melamine and products, not to detect other impurities in the real effects of interference, which can be true and reliable content of the data.
Melamine from food and animal feed, first using organic solvent extraction, the different types of food, a little bit different extraction methods, organic solvent extraction must be applied after solid phase extraction column. Done in the application of high performance liquid chromatography quantitative analysis of melamine, solid phase extraction column is the function of cleaning impurities, concentrated collection of melamine, such silica matrix C8 + SCX or SCX SPE column is preferred. On the other hand, in the application of liquid chromatography-mass spectrometry (LC-MS/MS) or GC (GC-MS) to do a quantitative analysis of melamine, cleaning impurities, remove medium effect is the SPE of the most important task, which When PSA or SCX SPE column is preferred.
Simple LC-MS/MS method is: Dairy, dairy food and livestock feed use of organic solvents such as acetonitrile extracted, 0.5mL extract through a PSA (500mg/3cc) solid phase extraction column (elution first with 5mL acetonitrile; leaching liquid thrown away), washing with 2ml acetonitrile, collecting all the outflow of liquid, with a constant volume of 1% formic acid. LC-MS/MS analysis of the sample directly.
Melamine LC-MS/MSMRM plan are as follows:
Milk and dairy products in melamine testing
LC-MS/MS test conditions: Column: InnovationTMWCX3um15cmx2.1mm Mobile phase A: acetonitrile (0.1% formic acid); mobile phase B: water (0.1% formic acid); flow rate: 300uL/min injection volume: 10uL;
Gradient: 55% A +45% B (isocratic)
Instrument: Perkin-Elmer200seriesHPLC ABIAPI4000tandemmassspectrometer LeapTechnologiesAutosampler Test sample: 100ng/mL melamine
MRM conversion (ESI positive ion mode): 127.2 85.20 (DP: 42; CE: 28; CXP: 5)
127.2 68.10 (DP: 42; CE: 42; CXP: 11)
127.2 110.30 (DP: 42; CE: 26; CXP: 8)
Melamine analysis in InnovationTMPFPPLC-MS/MS reservation is hydrophilic column chromatography mode is (hydrophilicInteractionchromatography). Acetonitrile is a weak solvent, water is a strong solvent. If you need to extend the retention time, simply increasing the ratio of acetonitrile. Column in the analysis of melamine InnovationTMPFPPLC-MS/MS good peak shape, no legacy effect, mass spectrometry and high sensitivity. Each extracted sample test time 4 minutes (5cm long PFPPLC-MS/MS column 1 minute, no complex peak interference. Use InnovationTMPSA or SCX SPE complete elimination of quantitative analysis of medium effects (Matrixeffect), you use the same mobile standard calibration curve with different brands, different areas, different components of milk and dairy products in melamine testing accuracy, fast, cheap, reliable. GLP certification that melamine recovery of 85-105%, CV <10%. because the extraction of the sample do not concentrate drying, LC-MS/MS analysis of 1-2 minutes can do 400-600 samples per day.
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