摘要[目的]探討電子煙煙液主要化學(xué)成分。[方法]建立了同時測定電子煙煙液中1,2丙二醇、薄荷醇、二甘醇、丙三醇和三甘醇含量的氣相色譜分析方法,并對19種電子煙品牌共計51種型號電子煙煙液進行含量測定。電子煙煙液經(jīng)超聲稀釋提取后,直接進行氣相色譜分析,采用內(nèi)標法定量
關(guān)鍵詞電子煙;1,2丙二醇;薄荷醇;二甘醇;丙三醇;三甘醇;氣相色譜
中圖分類號S572文獻標識碼A文章編號0517-6611(2014)24-08344-04
Simultaneous Determination of Main Chemical Components in Refill Liquids for Electronic Cigarettes by Gas Chromatography Method
HAN Shulei, HOU Hongwei et al(China National Tobacco Quality Supervision Test Center, Zhengzhou, Henan 450001)
Abstract[Objective] To figure out the main components of the refill solution for electronic cigarettes. [Method] A gas chromatography (GC) method for simultaneous determination of 1,2propylene glycol, menthol, diethylene glycol, glycerol and triethylene glycol of refill liquids for electronic cigarettes has been developed, and 51 samples of 19 different brands of ecigarette refill liquids were analyzed. Refill liquids were extracted and diluted with ultrasound before GC analysis and subsequent quantification by an internal standard method. [Result] 1,2propylene glycol, menthol, diethylene glycol, glycerol and triethylene glycol had good correlation coefficients (R2 more than 0.999), the average spiked recoveries ranged from 94.75% to 104.43% with a relative standard deviation lower than 4.96%, and the limit of detection is between 0.002 8% and 0.005 7%. The sample analysis showed that the concentrations of 1,2propylene glycol and glycerol in overwhelming majority of refill solutions were between 75% and 95%, that of menthol between 0% and 2.03% with 30.51% detected, and diethylene glycol and triethylene glycol were 3.4% and 5.1% detected of all, respectively. [Conclusion] It is concluded that this method has good sensitivity, reproducibility and recoveries, which can provide technical support for analysis of chemical components of electronic cigarettes.
Key wordsElectronic cigarettes; 1,2propylene glycol; menthol; diethylene glycol; glycerol; triethylene glycol; Gas chromatography
近年來,電子煙在全球銷量呈快速增長之勢[1-7]。1,2丙二醇和丙三醇除被用作傳統(tǒng)卷煙的保潤劑外[8],還被用作電子煙煙液的溶劑[9],雖然毒性很小,但消費者肺部對其長期持續(xù)吸入,其安全性尚未得到論證,且二者配比不同可能對煙液中煙堿遞送產(chǎn)生影響[4]。二甘醇和三甘醇作為煙草制品中受管制的保潤劑,有可能作為1,2丙二醇和丙三醇的雜質(zhì)或其他途徑被帶入煙液,而對人體健康帶來不利影響[10]。薄荷醇因其特殊的強烈薄荷香氣和涼爽味道,在電子煙產(chǎn)品中得到廣泛應(yīng)用,可改善電子煙的口感,但研究表明,在傳統(tǒng)卷煙中,薄荷醇可能增強消費者對卷煙的依賴,而提高肺癌的發(fā)病率,并與尼古丁代謝物有一定的相關(guān)性,增大了吸煙的危害性[11-12]。但是,對電子煙煙液中的1,2丙二醇、薄荷醇、二甘醇、丙三醇和三甘醇含量進行測定,卻鮮有文獻報道,如LPD公司用氣相色譜-質(zhì)譜聯(lián)用法測定了電子煙煙液中的1,2丙二醇、丙三醇含量,JeanFrancois用氣相色譜法測定了煙液中二甘醇、三甘醇含量,但都沒有進行方法驗證[9-10,13]。因此,亟待建立高通量的同時測定電子煙煙液中上述5種化合物含量的方法,并對其含量進行分析,為電子煙產(chǎn)品的化學(xué)成分測定提供技術(shù)支持。
1材料與方法
1.1材料
1.1.1研究對象。19種電子煙品牌共計51種型號電子煙煙液系網(wǎng)絡(luò)購買,為處于網(wǎng)絡(luò)銷量前列的品牌及型號,分別編號為1~51。
1.1.2主要試劑。1,3丁二醇(內(nèi)標,CAS:107880),1,2丙二醇(CAS:57556),薄荷醇(CAS:89781),二甘醇(CAS:111466),丙三醇(CAS:56815),三甘醇(CAS:112276),正十七碳烷(629787),1,4丁二醇(110634),純度>995%,美國Sigmaaldrich公司;甲醇,色譜純,美國TEDIA公司。
1.1.3主要儀器。SCION 456GC氣相色譜儀,配氫火焰離子化檢測器(GCFID),美國Bruker Daltonic公司;AE163電子天平(感量:0.000 1 g),瑞士Mettler公司;超聲波發(fā)生器,KQ700DB型數(shù)控超聲波清洗器。10~100 ml容量瓶,0.5~25 ml移液管等玻璃儀器。
1.2方法
3結(jié)論
該研究建立了同時測定電子煙煙液中1,2丙二醇、薄荷醇、二甘醇、丙三醇和三甘醇含量的氣相色譜分析方法,并對19種電子煙品牌共計51種型號電子煙煙液進行含量檢測。結(jié)果表明,該方法靈敏度高,重復(fù)性及回收率好,適合電子煙煙液中上述5種化合物的快速準確測定。實際樣品測試結(jié)果表明,1,2丙二醇和丙三醇是絕大多數(shù)電子煙煙液中的主要溶劑,近1/3的電子煙煙液中含有薄荷醇,但含量差異較大,且二甘醇和三甘醇皆有檢出。
參考文獻
[1] World Health Organization FCTC/COP/5/13,Electronic nicotine delivery systems,including electronic cigarettes,2012[EB/OL].http://apps.who.int/iris/bitstream/10665/77574/1/FCTC_COP5_13-ch.pdf.
[2] YANG L,RUDY S F,CHENG J M,et al.Electronic cigarettes:incorporating human factors engineering into risk assessments[J].Tob Control,2014,23(S2):47-53.
[3] DURMOWICZ E L.The impact of electronic cigarettes on the paediatric population[J].Tob Control,2014,23(S2):41-46.
[4] CHENG T.Chemical evaluation of electronic cigarettes[J].Tob Control,2014,23(S2):11-17.
[5] CHANG H.Research gaps related to the environmental impacts of electronic cigarettes[J].Tob Control,2014,23(S2):54-58.
[6] BROWN C J,CHENG J M.Electronic cigarettes:product characterisation and design considerations[J].Tob Control,2014,23(S2):4-10.
[7] VANSICKEL A R,EISSENBERG T.Electronic cigarettes:effective nicotine delivery after acute administration[J].Nicotine Tob Res,2013,15(1):267-270.
[8] 韓書磊,李中皓,陳歡,等.分散固相萃取-氣相色譜-質(zhì)譜聯(lián)用法同時測定卷煙煙絲中的3種保潤劑[J].煙草科技,2014(1):49-52.
[9] LPD Laboratory Services.Analysis of components from Gamucci electronic cigarette cartridges,tobacco flavor regular smoking liquid,2009[EB/OL].http://truthaboutecigs.com/science/11.pdf.
[10] ETTER J F,ZTHER E.SVENSSON S.Analysis of refill liquids for electronic cigarettes[J].Addiction,2013,108:1671-1679.
[11] CLARK P I,GAUTAM S,GERSON L W.Shortterm pulmonary effects of using an electronic cigarette[J].CHEST,1996,110(5):1194-1198.
[12] BROOKS D R,PALMER J R,STROM B L,et al.Menthol cigarettes and risk of lung cancer[J].Am J Epidemiol,2003,158(7):609-616.
[13] LPD Laboratory Services.Analysis of Chemical Components from High,Med Low Nicotine Cartridges,2008