柱后衍生高效液相色谱法对醛类化合物的水分析

2,4-DNPH柱前衍生化被认为是测量HPLC中醛的方法，但是，需要对样品进行预处理，如收集然后缩合或提取。JASCO介绍了一种以1,3-环己二酮为衍生化试剂，通过柱后荧光衍生化分析水中甲醛和乙醛的方法。UASGOApplication Note 2/3Application NoteWater Analysis for Aldehydes using Post-column Derivatization Water Analysis for Aldehydes using Post-column Derivatization by High Performance Liquid Chromatography It is a growing concern that aldehydes such as formaldehyde and acet a ldehyde may pollute air and water in lakes ， reservoirs， and rive r s in the environment . Therefore ， the aldehydes are subjected to regul a tions by Air Pollution Control ，Water Supply a n d Offensive Odor Control Acts in Ja p a n. Pre -column derivatizat i on with 2.4-DNPH is known as a method to measure aldehydes in HPLC， however， the pretreatment of samples such as collection then condensation or extraction is required. JASCO introduced a method for the analysis of formaldehyde and acetaldehyde in water by post-column f luorescence derivatization using 1，3- Cyclohexanedione as derivatization reagent which did not require such pretreatment . In this report， we extended the applicability of the method to other aldehydes by opt i mizing the derivatization conditions. Keyword： Aldehydes ， Formaldehyde，Acetaldehyde， 1，3-Cyclohexanedione， Post -column Derivatization， Shodex RSpak KC-8116E，Fluorescence detector Jasco PU-2080-CO2 App l ication L i brary： htt p ：//www.jascoi n c.com/a pplic a t i ons Experimental Equipment： Conditions： E l uent pump：PU-2080Column：Shodex RSpak KC-8116E (6.0Reagent pump：PU-2085mmlD x 250 mmL)Degasser ：DG-2080-53Eluent：3 mM Perchloric acid Autosampler ：AS-2057Flow rate：1.0 mL/min Column oven：CO-2060Reagent：1，3-Cyclohexanedione in ammonium acetate bu f ferReaction oven：RO-2061Reagent f low rate：0.4 mL/min Detector：FP-2020Column temp.：60°℃Reaction temp.：120℃Wavelength：Ex. 366 nm， Em. 440 nm，Gain x10 L Standard sample：Formaldehyde， Acetaldehyde 0.1mg/L each R esul t s Figure 1 s ho ws th e ch em ical r eac t i on o f 1，3-C y c lo h ex a n e di o n e with a ld e hy d es d u ri n g th e pos t -c o l umn d e r ivat i z at ion an d f ig u r e 2 s h ows f lo w p a t h o f t h e s y ste m. No .1： Eluent No .2 ： Degasser (DG-2080-53) No.3 ： Pump for eluent (PU-2080) No .4 ： Autosampler (AS-2057) No.5： Column oven (CO-2060)No .6： Column (Shodex RSpak KC-811 6E)No .7： Reagent No.8 ： Pump for reagent (PU-2085) No.9 ： Reaction oven (RO-2061) No.10： Reaction coil No.11： Cooling coil No.12： Fluorescence detector (FP-2020) No.13： Backpressure coil Fi g ur e 3 sh o ws c h r o m a t o gr am o f t h e s t an d a rd mix t u r e o f f o r mal dehyd e a n d ac e ta l d ehy de . The t wo c o mp o n en t s w e r e s eparat e d w i t hin 8 minu t e s. F i g ures 4， 5 a n d 6 s h ow ch r o m ato g ra m s of drin k i n g water， ri ve r wa t er and r a in wa t er， r es p ec t ively. The t o p c h r oma t o g ra m s a r e o f n eat s a m p l e s and th e b o tt o m on es a r e o f s a mp l es s p i ke d by a dd i n g 0.1 mg /L o f f o r ma l deh y de an d a c etal d e h yde. Al l of t h e sa m p l e s w ere se par a t e d . Fig ure 3. C h romato gr am of t h e stand ar d mixture o f formaldeh y de and acetalde h yde.1： F ormaldehyde ， 2： Acetalde h yde [0.1 mg/L e a ch 1 Figure 4. Chr o matog r am of d r i nk i ng wat e r.1： Formalde hy de， 2： Ace t aldehy de P re paration. Dr i nkin g water was f il t ered usi n g 0.45 p m m emb r an e f ilter. Fig ure 5. C h romato gr a m of r i ver water. 1： F ormaldehyde ， 2： Acetalde h yde Fig ure 6. Ch r omato gr am of rain water.1： Formalde h yde， 2： Ace t aldehyde P re parat i on . River water was f i ltered wi t h 0.45u m membran e f i l ter . P r e para t ion： Ra i n water wa s f i l tered wit h 0.45u m m embran e fil t e r .