固相萃取净化-离子色谱法测定不同生长期新鲜烟叶中的7种无机阴离子

Determination of 7 Inorganic Anions in Fresh Tobacco Leaves at Different Growth Stage by Ion Chromatography Method with Solid Phase Extraction Cleanup

为了研究不同生长期新鲜烟叶中无机阴离子的含量和变化规律,建立了一种固相萃取净化-离子色谱法测定新鲜烟叶中的,7种无机阴离子(F^(-)、Cl^(-)、Br^(-)、NO_(2)^(-)、NO_(3)^(-)、SO_(4)^(2-)、PO_(4)^(3-))的方法。样品经0.1 mol/L NaOH水溶液超声提取,萃取液经RP1.0cc固相萃取柱净化后,使用AS11-HC(4 mm×250 mm)色谱柱进行分离,以KOH为流动相,梯度洗脱。结果表明,7种无机阴离子在0.10~5.0μg/mL范围内具有较好的线性(r>0.996),检出限在0.01~0.04μg/mL,定量限在0.04~0.14μg/mL,加标回收率为96.3%~102%,相对标准偏差(RSD)在2.7%~4.8%。方法前处理操作简单,7种无机阴离子分离好,检测灵敏准确,可用于不同生长时期新鲜烟叶样品中多种无机阴离子含量的检测分析。

In order to study the content and the diversification of different inorganic anions in fresh tobacco leaves at different growth stage,a test method for separation and determination of seven inorganic anions(F^(-),Cl^(-),Br^(-),NO_(2)^(-),NO_(3)^(-),SO_(4)^(2-)and PO_(4)^(3-))was established by ion chromatography after solid phase extraction cleanup.The sample was extracted by ultrasonic with 0.1 mol/L NaOH aqueous solution,purified by RP1.0cc solid-phase extraction column.Then it was separated by AS11-HC(4 mm×250 mm)column,and eluted by gradient with KOH as mobile phase.The results showed that the seven inorganic anions had good linearity in the range of 0.10-5.0μg/mL(r>0.996),with the detection limit of 0.01-0.04μg/mL and the quantification limit of 0.04-0.14μg/mL.The recoveries were 96.3%-102%with the relative standard deviations(RSD)of 2.7%-4.8%.It could be found that the proposed method featured with the advantages of simple pretreatment,good separation effect,high sensitivity and accuracy.Therefore,it can be used for the determination of various inorganic anions in fresh tobacco samples at different growth stages.