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Determination of volatile carbonyl compounds in cigarette smoke by LC-DAD

机译:LC-DAD法测定卷烟烟雾中的挥发性羰基化合物

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摘要

An effective and rapid method, use of a 2,4-dinitrophenylhydrazine (DNPH)-treated Cambridge filter and high-performance liquid chromatography (HPLC) with diode-array detection (DAD), has been used for determination of low-molecular-mass carbonyl compounds in cigarette smoke. Different chromatographic mobile phases were investigated and the optimized mobile phase was a gradient prepared from water-acetonitrile-tetrahydrofuran (THF)-isopropanol, 59:30: 10:1 (v/v) (mixture A) and acetonitrile-water, 65:35 (v/v) (mixture B). Under the optimized chromatographic conditions, the 2,4-dinitrophenylhydrazones of formaldehyde, acetaldehyde, acrolein, acetone, propionaidehyde, 2-butanone, and iso-butyraldehyde were separated completely in an 18 min chromatographic run. The concentration of acid, which has large effect on carbonyl-DNPH derivatization, was investigated by adding different volumes of perchloric acid. The DNPH-treated Cambridge filter was convenient and effective compared with conventional methods used to collect and derivatize the carbonyl compounds present in cigarette smoke. Validation of the method showed it to be effective, precise, accurate, and linear over the range of concentrations of analyzed.
机译:一种有效,快速的方法,是使用经过2,4-二硝基苯肼(DNPH)处理的Cambridge过滤器和带有二极管阵列检测(DAD)的高效液相色谱(HPLC),用于测定低分子质量香烟烟雾中的羰基化合物。研究了不同的色谱流动相,最优化的流动相是由水-乙腈-四氢呋喃(THF)-异丙醇59:30:10:1(v / v)(混合物A)和乙腈-水65:30制备的梯度35(v / v)(混合物B)。在优化的色谱条件下,甲醛,乙醛,丙烯醛,丙酮,丙醛,2-丁酮和异丁醛的2,4-二硝基苯hydr在18分钟的色谱运行中被完全分离。通过添加不同体积的高氯酸,研究了对羰基-DNPH衍生化影响很大的酸浓度。与用于收集和衍生卷烟烟雾中羰基化合物的常规方法相比,经DNPH处理的Cambridge过滤器既方便又有效。方法的验证表明,该方法在所分析浓度范围内是有效,精确,准确和线性的。

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