食品中有毒害物质的分析.PPT

Choose View, Header and Footer to enter text here GC/MSD 或 HPLC-UV法 饲料中盐酸克仑特罗(Clenbuterol)的测定 盐酸克仑特罗(Clenbuterol) 盐酸克仑特罗是一种?肾上腺素兴奋剂，主要用于防治人，畜支气管哮喘和支气管痙挛，治疗剂量较低。 在饲料中添加盐酸克仑特罗具有营养再分配作用，提高饲料报酬，提高瘦肉率的效果。 盐酸克仑特罗在肌肉特别是在内脏中会有高浓度的残留，对人与动物的肝，肾及神经系统产生危害。 欧盟最早颁布法规禁止其作为饲料添加剂使用，美国和加拿大也禁用，我国农业部亦发文作出同样规定。 氨代亚硝基二甲胺 (N-Nitrosodimethylamine,NDMA) 仪器配置6890 GC - 5973 Mass Selective Detector with APEX ProSep 800 XT Plus Pre-separation Inlet and controller modules LVI（大体积进样）的参数控制 Experimental LVI （大体积进样）的优势 LVI 和化学电离质谱 PCI+SIM +LVI 技术分析NDMA NDMA分析的线性及重现性 结论 To demonstrate ProSep Function in Large Volume Injection using a simple 4 component mixture. 目的 The ProSep preseparation column was phase coated with HT-5, contained HT-5 coated fibers and a plug of silica wool in the upper 4-7 cm of the column. 6890 Plus GC with ALS made all injections onto 30m, .25 mm id, .25 um film HP-5 MS column …. MSD was operated in full scan, …. * LVI allows greater flexibility by providing the choice of – Lowered detection limits with an existing extraction methodology OR Less Sample Prep / Extraction while maintaining required detection limits ProSep has applications demonstrating both approaches and others (e.g., derivatization “during injection”, …) * = 提高选择性和灵敏度 20 attograms / ul of Octafluoronaphthaleneacquired using LVI with ECNI – MS on 5973 (44,000 molecules / ul ) * 20 fg/uL 200 fg/uL PCI-NH3-SIM chromatograms of 50 uL injections of NDMA standards in CH2Cl2 . Applying a concentration recovery factor of 500, 200 fg/ul = 0.4ng/l (0.4 ppt) 20 fg/ul = 0.04ng/l (40 ppq) * NDMA quantitation curve from 20 fg/ul to 4000 fg/ulr2 =0.999 Reproducibility in 75/92 m/z ratio and response (n=5)for concentrations of NDMA from 20 to 4000 fg/ul * Apex ProSep Preseparation Inlet Behaves as a Chromatographic Zone Inlet System Performs separations in Large Volume Inlet modes Increased analytical integrity, lowered column and detector maintenance, etc.. Work with authentic samples and a wide