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    离子色谱法测定再造烟叶中山梨酸根、磷酸根和柠檬酸根的含量

    IC Determination of Sorbate, Phosphate and Citrate in Reclaimed Tobacco

    • 摘要: 称取再造烟叶样品0.150 0 g,加水50.0 mL并振荡提取20 min,使样品中的山梨酸根、磷酸根和柠檬酸根溶入水中。所得溶液通过0.45 μm滤膜过滤。滤液用0.25 mol·L-1 NaOH溶液调节其酸度至pH 11.0。取此溶液5 mL通过经活化的反相柱净化。弃去前3 mL流出液,收集其后的2 mL流出液,进行离子色谱分析。选用AS11-HC色谱柱为固定相,进样量为50 μL,用KOH溶液作为流动相在不同的时间段流经色谱柱进行梯度洗脱。采用自循环抑制电导检测器测定。测得山梨酸根的线性范围在0.2~4.0 mg·L-1之间,磷酸根和柠檬酸根的线性范围均在2.0~40 mg·L-1之间,其检出限(3s)依次为0.022,0.015,0.010 mg·L-1。按此方法分析3件实样,3种酸根测定值的相对标准偏差(n=5)在0.18%~0.74%之间。在此3个样品的基础上,加入标准溶液进行回收试验,测得回收率在97.3%~103%之间。

       

      Abstract: The reclaimed tobacco sample (0.150 0 g) was extracted by oscillation for 20 min with 50.0 mL of water to dissolve sorbate, phosphate and citrate from tobacco into water. The solution was filtered through 0.45 μm filtering membrane, and the acidity of the filtrate was adjusted to pH 11.0 with 0.25 mol·L-1 NaOH solution. An aliquot of 5 mL of the filtrate was purified by passing through activated RP column. The first 3 mL of the eluate from the RP column were discarded and the latter 2 mL were collected for IC analysis. AS11-HC chromatographic column was chosen as stationary phase and 50 μL of the purified sample solution was introduced for IC separation. KOH solution was used as mobile phases passing through the column at various definite time intervals for gradient elution. Self-cyclic inhibition conductance detector was used for determination. Linearity ranges found were between 0.2-4.0 mg·L-1 for sorbate, and between 2.0-40 mg·L-1 for phosphate and citrate, with their detection limits (3s) of 0.022, 0.015, 0.010 mg·L-1 respectively. 3 substantial samples were analyzed by the proposed method, giving values of RSDs (n=5) in the range of 0.18% to 0.74%. On the base of the 3 samples, standard solutions were added and analyzed by this method to test for recovery, giving results of recovery in the range of 97.3% to 103%.

       

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