色谱柱后衍生高效液相色谱法分析醛类化合物

智能文字提取功能测试中

甲醛和乙醛等醛类物质是一种环境污染物，可能会污染大气、湖泊、沼泽、水库和河流，这正成为人们关注的焦点。因此，醛类受到各种法规的约束。作为一种使用HPLC测量醛类的方法，2，4-DNPH柱前衍生法是众所周知的，但这需要在分析前进行预处理，如样品收集、缩合和提取。JASCO介绍了以1,3-环己烷二酮为衍生化试剂，采用柱后荧光衍生化法对甲醛和乙醛进行分析，该方法不需要预处理。USGOApplication Note 2/4Application NoteAnalysis of Aldehydes using Post-column Derivatization Analysis of Aldehydes using Post-column Derivatization by High Performance Liquid Chromatography It i s becoming a big concern that aldehydes such as the formaldehyde and acetaldehyde act as an environmental pollutan t that may contaminate the atmosphere， lakes， marshes， reservoirs， and r i vers. Therefore ， aldehydes are subject to various regulations like the Air Pollut i on Control Law， Water Supply Law， and Offensive Odor Control Law i n Japan. As a m e t hod to measure ald e hydes using HPLC， the pre -column derivatization method by 2，4-DNPH is well known ， but this requires pretreatment such as sample collec t ion， condensation and extra c tion before analysis . JASCO has introduced the analysis of formaldehyde a n d acetaldehyde by the post column f l uorescence derivat i zation method using 1，3- Cyclohexanedione as a derivatizing reagent which doesn't need such pretreatment . The two above mentioned aldehydes and three others， propyl ald e hyde， butyraldehyde， and valeraldehyde were analyzed simultaneous l y. Keyword： Aldehyd e s ， 1，3-Cyclohexanedione， Post column derivat i zation method， Shodex RSpak KC-8116E，Fluorescence de t ector Jasco CO2 Delivery Pump：PU-2080-CO2 Experimental Equipment： Conditions： Eluent pump： PU-2080 Reagent pump： PU-2085 Degasser： DG-2080-53 Autosampler： AS-2057 Reaction oven： RO-2061 Detector： Column： Shodex RSpak KC-811 6E (6.0 mmlDx250 mmL) Eluent： 3 mM Perchloric acid Flow rate： 1.0 mL/min Reagent： 1，3-Cyclohexanedione in ammoniumacetate buffer Reagent flow rate： 0.4 mL/min Column temp.： 60°C Reaction temp.： 120°C Wavelength： Ex. 366 nm， Em.440 nm， Gain x10 100pL Injection volume： Standard sample： Formaldehyde， Acetaldehyde， Propylaldehyde， Butylaldehyde， Valeraldehyde 0.1 mg/Leach Results In fig ur e 1， the 1，3-C y clo h e x a n e di on e r e a c t i on d u ri n g the p o s t c ol u m n der iva t i z a ti o n me th o d i s sh o wn a n d fi g ur e 2 i l lu s t r at es flow di agr a m for th e HP L C . Fi g u r e 1. 1，3-C yc l o h e x anedi o ne r eact i on f o rm u l a o f pos t c ol um n de r iva t i za t ion m et h o d F i g u r e 2. F l ow s y ste m diag r a m N o.1： E lu e n t No.7： R eag en t No .2 ： D e g ass e r (DG -2080-53)No.8 ： P ump f o r re a g e nt (PU-2085)N o.3 ： P u m p f o r elu e nt (P U-2080)N o.4 ： Au t os a mpl e r (AS-2057)N o .5 ： C o lum n o ve n (C O -2060)No.11： Co ol i ng c o i l N o.6 ： C o lumn (S ho d ex R S p a k K C-811 6E) No.9 ： R eac t i o n o v e n (RO-2061)No.10： Re a ct io n co i l No.12： Flu ores c e nc e d e t e c t o r (FP-2020)No.13： Backpressure coi l Fi g u re 3 sh o w s t h e c hr om a t o g r a m o f 5 a l d eh yde s. As s h o wn ， th e 5 c omp o n en t s we r e c l ear l y s e p a r a t e d wi thi n 16 m in. Th e m i ni m um d et e c t able a mou n t (i n c as e o f S/N=3) o f e a c h c om po ne n t is a s b e l o w . Fi g ur e 3. Ch r om a to gram o f 5 a l dehyd e s a nd mi n i m u m d e tec t able a m ou n t of eac h.1： For m a l dehyd e (0.091 n g)， 2：A c e t a l de h yd e (0.105 n g )， 3： P rop y l a l de h yd e (0.418 n g )， 4： B u t yla l dehyd e (0.593 n g )， 5： Val e r a lde hyde (4.53 ng )