FDA 三聚氰胺的检测方法.docVIP

GC-MS Screen for the Presence of Melamine and Cyanuric Acid(formerly titled GC-MS Screen for the Presence of Melamine) (Adapted from FDA/ORA Forensic Chemistry Center SOP T015) Title Revised April 25, 2007 PURPOSE: This procedure provides a general guide for the sample preparation and analysis of wheat gluten and pet food matrices for melamine using gas chromatography/mass spectrometry.? This procedure is designed to screen the TMS derivative of a methanol extract of the sample and it incorporates instrumental parameters which permit 10.5 minute run times. SCOPE: This procedure is applicable to dry wheat gluten, dry pet food, and wet “cuts and gravy” type pet food.? This procedure involves extractions in methanol and therefore preselects compounds which are soluble or partially soluble in methanol.? Due to solubility limitations of melamine in methanol, this method is intended to be a qualitative screen only. RESPONSIBILITY: It is the responsibility of the analyst to note any modifications to this procedure in the worksheet. DEFINITIONS AND ACRONYMS: TMS – trimethylsilyl SAFETY CONSIDERATIONS: Accepted safety measures should be employed when working with chemicals and pressurized gases. EQUIPMENT: Agilent 5975 GC-MS system equipped with a 30m DB-5MS column (or equivalent)Reacti-Vap – Evaporating/Heating Module REAGENTS: Methanol: HPLC gradePyridine: Certified A.C.S.BSTFA with 1% TMCS: bis(trimethylsilyl)trifluoroacetamide with 1%Trimethylchlorosilane (e.g. Sylon BFT, Supelco) QC ELEMENTS: A blank should be run at the onset of each analysis and then randomly throughout the analysis if there is suspicion of carryover.? A fortified sample (see Part C) should be analyzed with each set of samples to demonstrate effective system performance. PROCEDURES (PROCESS DETAILS): This procedure may be used with the GC operating in either the splitless or split (1:20) mode.? Generally, the splitless mode is advisable for samples where more sensitivity is required.?? The split