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在线固相萃取-离子色谱法测定再造烟叶浆料中的17种有机酸

Quantification of 17 organic acids in reconstituted tobacco slurry by online solid phase extraction-ion chromatography

  • 摘要: 为测定再造烟叶浆料中有机酸的浓度,利用过滤、离心、在线固相萃取净化和浓缩样品,通过离子色谱阀切换、二元梯度泵清洗再生净化柱,高压泵分离AS11-HC离子色谱柱中的有机酸,建立了同时测定再造烟叶浆料中17种有机酸的在线净化离子色谱法。结果表明:①17种有机酸在0.5~10.0 μg/mL范围内线性关系良好,相关系数均大于0.999,方法检出限为0.002~0.400 μg/mL,定量限为0.010~0.900 μg/mL。②在2、4、6 μg/mL 3个加标水平的平均回收率为90.5%~117.1%,相对标准偏差为0.4%~4.4%。17种有机酸日内、日间测定结果的变异系数分别在0.59%~2.57%、0.72%~4.80%之间。该方法操作简便、可靠、重复性好,可用于再造烟叶浆料中有机酸的测定。

     

    Abstract: In order to quantify the contents of organic acids in reconstituted tobacco slurry, an online purification ion chromatography method for simultaneously analyzing 17 organic acids was established by adopting filtration, centrifugation, online solid phase extraction purification and concentration of samples. The purification column was regenerated by ion chromatography valve switching and binary gradient pump cleaning, and the organic acids were separated in an AS11-HC ion chromatographic column with a high pressure pump. The results showed that: 1) The linearities of 17 organic acids were satisfactory in the range of 0.5-10.0 μg/mL with the correlation coefficients all higher than 0.999; the limits of detection were 0.002-0.400 μg/mL, and the limits of quantification were 0.010-0.900 μg/mL. 2) The average recoveries at the spiked levels of 2, 4 and 6 μg/mL were in the range of 90.5%-117.1%, and the relative standard deviations (RSDs) were 0.4%-4.4%. The coefficients of variation for intra- and inter-day determination of the 17 organic acids ranged from 0.59% to 2.57% and from 0.72% to 4.80% respectively. This method is simple, reliable and repeatable, and can be used for analyzing the organic acids in reconstituted tobacco slurry.

     

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