高效液相色谱柱后衍生法分析空气中的甲醛

甲醛和乙醛等醛类作为环境污染物可能污染大气、湖泊和沼泽、水库和河流等环境，这已成为人们关注的焦点。因此，它受到各种法规的监督。作为一种使用高效液相色谱法测量大气中醛类的方法，通常采用的方法是使用包封含有2,4-DNPH的硅胶的采样器收集大气中的醛类，并用acetonitrile 提取收集后衍生的醛类。JASCO介绍了以1,3-环己烷二酮为标记试剂，采用柱后荧光衍生法对甲醛和乙醛进行分析。这种方法用于分析大气中的醛类。结果，成功地分析了水萃取大气中的醛类物质以及水中醛类物质的来源。Application Note 2/4Application NoteAnalysis of Formaldehyde in Air using Post-column Derivatization Analysis of Formaldehyde in Air using Post-column Derivatization by High Performance Liquid Chromatography It is becoming a big concern that aldehydes such as the formaldehyde and acetaldehyde as an environmental pollutant may contaminate the environment such as the atmosphere， l akes and marshes， reservoirs， and rivers. Therefore， it i s monitored under various regul a tions like Air Pollution Control Law， Water Supply Law， and Offensive Odor Control Law in Japan. As a m et h od to measure aldehydes in the atmosphere using HPLC ， the general method employed is to collect ald e hydes in t h e atmosphere using the sampler enc l osing silicagel containing 2，4- DNPH and extracting aldehydes derivatized after co l lection by the acetonitrile. JASCO has i ntroduced the ana l ysis of formaldehy d e and aceta l dehyde by the post column fluorescence derivatization method using 1，3-cyclohexanedione as a l abeling reagent . This method is used to analyze aldehydes in the atmosphere. As a result ， aldehydes i n the atmosphere extracted by water were analyzed successfully as well as the source of aldehydes in water . Keyword ： Aldehy d es， Passive gas tube，1，3-Cyclohexanedione， Post column derivatization method， Shodex RSpak KC-811 6E， Fluorescence detector Jasco PU-2080， DG-2080-53，LG-2080-02，AS-2055，CO-2060，UV-2070 Experimental Equipment： Conditions： El u ent pump：PU-2080Column：Shodex RSpak KC-811 6E (6.0 mmlD Reagent pump：PU-2085x250 m mL)Degasser：DG-2080-53Eluent：3 mM Perchloric acid A 2057Futosamlow rapler ：AS -te：1.0 mL/mi n Column oven ：CO-2060Reagent ：1，3-Cyclohexanedione i n ammon i um acetate buffer Reaction oven ：RO-2061Reagent flow rate ：0.4 mL/min Detector ：FP-2020Colum n temp.：60°C Reaction temp.：120℃Wavelength：Ex. 366 nm， Em. 440 nm ， Gain x10Inject i on vol u me：50 pL Standard sample：Formaldehyde 0.1 mg /mL R e sults In fig ur e 1， t h e 1，3-cy c l oh e x a n e d i o n e r eac ti o n durin g th e p o s t co lum n deriv a t iza t ion m eth o d is s h o wn a n d f i g u r e 2 il l u s tr a t e s syst e m f l o w d i a gr a m. Figur e 1. 1，3-C yclo h exanedione rea c ti o n dur i n g t h e p ost column d e rivati z a t ion m e t hod. Figure 2. Flow system diagram No.1： E lu en t N o .8 ： P u mp fo r r e a g e n t (PU-2085)No.2 ： De g a ss er (D G -2080-53)No .9 ： R e a c tion o v e n (R O -2061)No.3 ： P ump for el u e nt (PU-2080)No .10： Re a ction c oil No.4 ： A u t o sa m pl er (A S -2057)N o .11： C o o l ing c o i l No.5 ： C ol u m n o ve n (C O -2060)No .12： Fl u o r esc e n c e d e t e ct or (F P -2020)No.6 ： C o l u m n (Sho d e x R S pa k KC -811 6E )No .13： Ba c kp r e ss u r e c oi l No.7： Re a g en t Adsorption agent (TEA i mpregnated silica gel) Figure 4. Ext r act i on m et h o d f r o m passive gas tube Fi g u r e 5 sh o w s t h e c hr oma t o gram of th e sa mp l e i n th e l abo r at o r y a t mos p h e re c oll e c t e d b y th e p a s s i v e ga s t u b e . Th e ca l c u l at e d c on c en t r a ti o n o f for m a l deh y d e ob t a i n e d was 0.0054 mg /L.