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水分散-DNPH衍生-LC-MS/MS法同时测定电子烟液中8种羰基物

Simultaneous quantification of eight carbonyls in e-liquids using water dispersion and 2, 4-dinitrophenylhydrazine derivatization combined with LC-MS/MS

  • 摘要: 为分析电子烟液中的羰基物,建立了同时测定电子烟液中甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮和丁醛8种羰基物的LC-MS/MS法。电子烟液中的羰基物在酸性条件下与2, 4-二硝基苯肼(DNPH)反应生成腙类化合物,对比了LC-MS/MS法和HPLC法对检测结果的影响,考察了溶剂背景和反应体系均一性,优化了DNPH浓度、酸性溶液浓度和反应时间参数,并考察了衍生液的稳定性。结果表明:①电子烟液基质复杂,LC-MS/MS法灵敏度高、选择性好,可消除基质干扰;②与甲醇相比,乙腈产生的背景较小,选择乙腈配制DNPH溶液;③在电子烟液中加入水作为分散剂,可提高甘油高含量样品溶液的均一性;④在衍生液中加入吡啶,改善了衍生化产物的稳定性;⑤8种羰基物的相关系数均大于0.999,定量限在17~93 ng/g之间,3个加标水平的回收率在92.5%~106.4%之间,日内和日间精密度分别为3.2%~6.2%和4.1%~7.9%,表明该方法线性良好、灵敏度高、精密度好。该方法前处理过程简单、快速,适合大批量电子烟液样品的检测。

     

    Abstract: In order to analyze the carbonyls in e-liquids, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to simultaneously determine eight carbonyls in e-liquids, including formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butanone, and butyraldehyde. The carbonyls in e-liquids reacted with 2, 4-dinitrophenylhydrazine (DNPH) forming hydrazone derivatives under acidic conditions. The analysis results of carbonyls by LC-MS/MS and HPLC methods were compared, and the solvent background and uniformity of reaction system were investigated. After optimizing DNPH concentration, acid solution concentration and reaction time, the stability of derivative solution was studied. The results showed that: 1) The interference of complex e-liquid matrix could be eliminated by using LC-MS/MS method due to its high sensitivity and good selectivity. 2) Compared with methanol, acetonitrile presented a smaller solvent background and was chosen to prepare DNPH solution. 3) The homogeneity of sample solution with high glycerol content was improved by adding water as dispersant in e-liquid. 4) The stability of hydrazone derivatives was improved by adding pyridine in derivative solution. 5) The correlation coefficients of the eight carbonyls were more than 0.999 in corresponding concentration ranges, LOQs were between 17-93 ng/g, and the spiked recoveries ranged from 92.5% to 106.4% with intra- and inter-day RSDs in the ranges of 3.2%-6.2% and 4.1%-7.9% respectively. This method is suitable for determining large quantities of e-liquid samples with better linear, high sensitivity and precision, simple and fast pretreatment.

     

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