乳制品中三聚氰胺的高效液相色谱快速分析

三聚氰胺是一种有机氮化合物，其结构中心有一个三嗪环。它被用作三聚氰胺树脂的材料，具有很高的耐热性和耐水性，用于机械加固。最近，有案例表明，三聚氰胺被用作稀释牛奶的添加剂，以弥补蛋白质含量不足的问题，但这种牛奶产品引起了健康问题。美国食品药品监督管理局（FDA）一直在评估三聚氰胺的风险，并指定紫外检测高效液相色谱法作为食品中三聚氰胺的分析方法之一。UASGOApplication Note 2/4 High Speed Analysis of Melamine in Dair y Melamine is an organic nitrogen compound which has a triazine r i ng in the center of i ts structure. It is used as the mate r ial of melamine resin which has high thermal and water resistance a n d is used for mechanical strengthening.Recently， there was a case that melamine was used as an addit i ve to diluted mi l k to make-up for the l a ck protein content ， however， this m ilk product cause d health problems. The Food and Drug Administrat i on (FDA) has been evaluating the risk of melamine and has assigned HPLC with UV detection as one of the analysis methods of melamine in food. In this paper， the analysis results of melamine in a m ilk product was measured using a PDA detector. Application Note Hi gh S pee d Ana l y s i s of M e l ami n e i n D a i r y P r o d uc t s b y H P L C E xperimenta l Equipment Co nd i t i ons Pump： PU-2089 Column oven： CO-2065 Autosampler： AS-2057 Detector： MD-2018 Column： ZORBAX RX-C8 (4.6 mmlDx 150 mmL， 5 um) Eluent： 10mM Citric acid， 10mM Sodium-1-octanesulfonate in Water/Acetonitrile/Methanol (85/7.5/7.5) Flow rate： 1.0 mL/min Column temp.： 40℃ Wavelength： 200-400nm Injection volume： 10 pL Standard sample： Melamine 10 mg/mL in Water Resu l ts Figu r e 1 shows t h e str u ct u re o f melamine， w h ile fig ur e 2 sh o ws t h e c h r o matogram a n d co nt ou r pl ot of me l am in e. Figure 1 Structure of melamine Fi g ure 2. S p ect r u m of pi p e r in e s a mpl e Figu r e 3 shows t h e on peak spectrum of the me l amine standard samp l e . Figure 3 On pe ak spe c tr u m o f t h e m ela m in e s t a n dar d s a mpl e Figu r e 4 shows t h e ch r oma t ogra m a n d on peak s p ectru m o f m ilk spiked w ith melam in e . B y r egister i ng t he spe c t r u m of t h e sta n da rd sample i n figure 3， t h e cor r ela t io n coe f fic i en t was calculated to be 1.000. F i gure 4 C hr o ma to gram o f m ilk s p i k e d with mel amin e. S a m pl e pre p a r at i o n ： 20 p L o f 100 pg /L m el am in e so l u ti on wa s a d ded to 180 pL o f m ilk ， d il u ted wi t h 1800 p L of u ltrap u re water an d a dded to 200 pL o f e luent . The s o l u tion was c entri fu ge d at 5000 rpm f o r 10 m inu t es an d t h e n t h e s up e r n at a n t wa s f iltr ate d u si n g 0.45 pm m e mbr an e f ilter .