HQ-DNPH 3 V SBT 2003 WHO 2,4- Report Series DNPH 8 HQ-DNPH cartridge DNPH. HQ-DNPH cartridge 2 1 HPLC LC-20AD SPD M20A

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1 BUNSEKI KAGAKU Vol. 6, No. 1, pp The Japan Society for Analytical hemistry 791 2, HQ 2,4- DNPH HQ-DNPH, 3 V 1 SBT 23 WHO Technical Report Series FDA : : α,β- 26 Feng 7 21 Uchiyama α,β- HQ 2,4- DNPH 8 HQ-DNPH cartridge 9 HQ DNPH α,β- HQ-DNPH cartridge HPL L-2AD SPD M2A

2 792 B U N S E K I K A G A K U Vol Fig. 1 Schematic drawing of the HQ-DNPH-cartridge Prominence L-2 Ascentis Express RP-Amide 2.7 μm particle size, 15 mm 4.6 mm i.d., Supelco 4 1 μl HPL 4 6 A 5 mmol/l B.7 ml/min A B 1 15 B 1 G/MS 589/5972 SLB-5ms.25 mm i.d. 3 m.25 μm /min 3 26 m/z 4 35 G MS EI 7 ev 2 min Borgwaldt Technik GmbH model LM1/PLUS HI Health anada Intensive 1 55 ml HPL Millipore Milli-Q 2, AG SI-Tech 6/8 mesh 12 Å 1 A, B,, D, E, F, G, H, I, J 2 2 DNPH-cartridge HQ-cartridge DNPH-cartridge : DNPH-cartridge 5 g 5 ml 3 5 ml 2 5m L 2 2,4-.25 g 1 g 1 ml 3 ml 4 DNPHsilica 28 mg 1 ml DNPH-cartridge HQ-cartridge :.5 g 5 ml 5 g 4 HQ-silica 28 mg 1 ml HQ-cartridge 2 3 DNPH-cartridge HQ-cartridge HQ- DNPH-cartridge Fig. 1 HQ-DNPHcartridge HQ-cartridge DNPH-cartridge HI HQ-DNPHcartridge DNPH-cartridge HQ-cartridge HQ-DNPH-cartridge DNPH-cartridge 1 4 ml 1 1 ml 1 μl HPL DNPH A J HQ-DNPH Fig. 2 DNPH 1 3 DNPH WHO 11.1 mg/m 3 A J 11, 13, 4.6,.3, 1.6, 2, 8.1, 2.8, 6.9,.5 mg/m 3

3 : HQ DNPH 793 absorbance at 36 nm FA AA FA: formaldehyde AA: acetaldehyde AR: GO: MGO: AR GO MGO Fig. 2 Representative chromatogram of carbonyl- DNPH derivatives generated from electronic cigarette F 2 mg/m 3 26 mg/m 3.1 mg/m 3 D, E, J A, B,, D, E Fig A, formaldehyde A, A, A, B, formaldehyde B, B, B, , formaldehyde , , , D, formaldehyde D, D, D, E, formaldehyde E, E, E, Fig. 3 oncentrations of formaldehyde,, and generated from various brands of electronic cigarettes

4 794 B U N S E K I K A G A K U Vol A 1 No.7 No No B 1 No.2 No.3 No.7 No.8 No.9 5 A 97 mg/m 3 A 1 No.1 No.8 D mg/m 3 E HQ-DNPH 1.9, 1.8, 1.2, : F, G, H, I DNPH HPL : F, G, H, I 2 3 G/MS μl HQ-DNPH-cartridge Uchiyama 9.5 L/min V Fig. 4 FA AA AR GO MGO Scheme 1 Fig

5 : HQ DNPH FA Ethylene glycol FA AA Propylene glycol FA Glycerol AR.1 GO MGO AA absorbance at 36 nm.1 MGO absorbance at 36 nm.1 GO AA absorbance at 36 nm Fig. 4 hromatographic profiles of carbonyl compounds generated by heating ethylene glycol (left panel), propylene glycol (middle panel) and glycerol (right panel) H O H 2 OH O 2 + 2H 2 O H 2 OH H O ethylene glycol H 2 OH H O O 2 H OH + 2H 2 O H 2 H H3 O propylene glycol H H 2 OH O H OH H + 2H 2 O H 2 OH H 2 glycerol Scheme 1 Formations of aldehydes from glycerol and glycols 3 V 4 5 V V

6 796 B U N S E K I K A G A K U Vol ethylen glycol formaldehyde acetaldehyde 15 1 propylene glycol formaldehyde acetaldehyde 15 1 glycerol formaldehyde acetaldehyde ethylen glycol propylene glycol glycerol Fig. 5 Generation of carbonyl compounds from ethylene glycol, propylene glycol and glycerol heated by using a Nichrome wire H ) World Health Organization : WHO Technical Report Series, No. 955, The Scientific Basis of Tobacco Product Regulation, Third Report of a WHO Study Group, 955, (21). 2) U.S. Food and Drug Administration, FDA and Public Health Experts Warn About Electronic igarettes : FDA News Relese, July 22, (29). 3) G. McGwin, J. Lienert, J. I. Kennedy : Environ. Health Perspect., 118, 313 (21). 4) R. Golden, D. Pyatt, P. G. Shields : rit. Rev. Toxicol., 36, 135 (26). 5) National Toxicology Program : Final Report on arcinogens Background Document for Formaldehyde. Rep. arcinog. Backgr. Doc , i-512 (21). 6) T. Salthammer, S. Mentese, R. Marutzky : hem. Rev., 11, 2536 (21). 7) Z. Feng, W. Hu, Y. Hu, M. S. Tang : Proc. Natl. Acad. Sci. USA, 13, 1544 (26). 8) S. Uchiyama, Y. Inaba, N. Kunugita : J. hromatogr. B, 879, 1282 (211). 9) S. Uchiyama, Y. Inaba, N. Kunugita : J. hromatogr. A, 1217, 4383 (21). 1) Health anada, Method T-115, Determination of Tar, Nicotine and arbon Monoxide in Mainstream Tobacco Smoke, (1999), (Ottawa, anada). 11) World Health Organization (WHO) Regional Office for Europe, Air quality guidelines for Europe, WHO Regional Publications, European Series, No. 23, (1987).

7 : HQ DNPH 797 Determination of arbonyl ompounds Generated from the Electronic igarette Using oupled Silica artridges Impregnated with Hydroquinone and 2,4-Dinitrophenylhydrazine Kazushi OHTA 1, Shigehisa UHIYAMA 2, Yohei INABA 2, Hideki NAKAGOME 1 and Naoki KUNUGITA 2 1 Graduate School of Engineering, hiba University, 1-33, Yayoicho, Inage-ku, hiba-shi, hiba Department of Environmental Health, National Institute of Public Health, 2-3-6, Minami, Wako-shi, Saitama (Received 25 May 211, Accepted 4 July 211) The electronic cigarette, introduced recently to the marketplace, is a battery-powered device that provides tobacco-like smoke by heating a chemical solution into a vapor. There is, however, little information available regarding the safety of the electronic cigarette, because analysis of the smoke produced is very difficult due to the nature of the chemical components, e.g. and other carbonyls. Recently, an effective method for the determination of and other carbonyls using a dual-cartridge system has been developed. Each cartridge consists of reagent-impregnated silica particles ; the first contains hydroquinone (HQ) for the inhibition of polymerization, while the second contains 2,4-dinitrophenylhydrazine (DNPH) for the derivatization of carbonyls. Samples were drawn through the cartridge, first through the HQ-impregnated silica and then the DNPH-impregnated silica. During extraction, excess DNPH was washed into the HQ bed, where it reacted with and other trapped carbonyls to form the corresponding hydrazone derivatives. All of the hydrazones derived from airborne carbonyls were completely separated and measured using HPL. In this study, we analyzed carbonyl compounds generated by the electronic cigarette using the HQ-DNPH technique. Results showed that formaldehyde, acetaldehyde,, and methyl were contained in the electronic cigarette smoke. The maximum concentration of formaldehyde was 26 mg/m 3. Depending on the brand, cartridges usually contain humectants to produce the vapor (e.g. ethylene glycol, propylene glycol or glycerol) and flavors (e.g. tobacco, mint, fruit and chocolate). Therefore, a simple electronic cigarette was made, comprising a coiled Nichrom wire and glycols ; a voltage of V was applied to the Nichrom wire. It was found that when the voltage exceeded 3 V, a mist containing carbonyl compounds was generated. From the results, it was elucidated that ethylene glycol was oxidized to formaldehyde and ; propylene glycol was oxidized to formaldehyde, acetaldehyde and ; and glycerol was oxidized to formaldehyde,, and. Keywords : electronic cigarette ; hydroquinone ; 2,4-dinitrophenylhydrazine ; ; carbonyl compounds.