HPLC Determination of 3 Polyamines in Fresh Tobacco Leaves
摘 要
新鲜烟叶样品经0.4 mol·L-1高氯酸溶液超声提取,以4 g·L-1的丹磺酰氯丙酮溶液为衍生化试剂,在40℃下衍生40 min,采用高效液相色谱法测定样品溶液中腐胺、亚精胺、精胺等3种多胺的含量。以ZORBAX SB-C18色谱柱(4.6 mm×150 mm,5 μm)为分离柱,用0.01 mol·L-1乙酸铵溶液和乙腈以不同比例混合的溶液为流动相进行梯度洗脱,用二极管阵列检测器测定。3种多胺的质量浓度均在0.50~50.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.07~0.08 mg·L-1,测定下限(10S/N)为0.23~0.28 mg·L-1。方法用于新鲜烟叶样品的分析,加标回收率为86.4%~100%,测定值的相对标准偏差(n=6)为0.70%~4.4%。
Abstract
The fresh tobacco leave sample was extracted ultrasonically by 0.4 mol·L-1 HClO4 solution, and then derived with using 4 g·L-1 dansulfonyl chloride acetone solution as derivating reagent at 40℃ for 40 min. HPLC was applied to the determination of 3 polyamines, i.e. putrescine, spermidine and spermine in the sample solution. ZORBAX SB-C18 chromatographic column (4.6 mm×150 mm, 5 μm) was used as separation column with mixtures of 0.01 mol·L-1 ammonium acetate solution and acetonitrile with different mixing ratios as mobile phase in the gradient elution, and photodiode array detector was used for determination. Linear relationships between values of peak area and mass concentration of 3 polyamines were kept in the same range of 0.50-50.0 mg·L-1, with detection limits (3S/N) in the range of 0.07-0.08 mg·L-1 and lower limits of determination (10S/N) in the range of 0.23-0.28 mg·L-1. The proposed method was applied to the analysis of samples of fresh tobacco leaves, giving values of recovery found by standard addition method and RSDs (n=6) of determined values in the ranges of 86.4%-100% and 0.70%-4.4% respectively.[WT5HZ]
中图分类号 O652.63 DOI 10.11973/lhjy-hx202010006
所属栏目 工作简报
基金项目 中国烟草总公司重大专项[110201901016(JY-03)];云南中烟工业有限责任公司重点项目(2018JC06)
收稿日期 2020/1/6
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备注黄丽佳,硕士研究生,主要从事仪器分析、色谱分析工作
引用该论文: HUANG Lijia,LIANG Mengjie,LI Yingjun,MI Qili,HUANG Haitao,br,YANG Yekun,YANG Guangyu,LI Jing. HPLC Determination of 3 Polyamines in Fresh Tobacco Leaves[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(10): 1079~1084
黄丽佳,梁梦洁,李应郡,米其利,黄海涛,杨叶昆,杨光宇,李晶. 高效液相色谱法测定新鲜烟叶中3种多胺[J]. 理化检验-化学分册, 2020, 56(10): 1079~1084
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【23】孙艳妮,张宁,王翠玲,等.高效液相色谱法鉴别及测定重要吴茱萸中的生物胺[J].分析化学, 2014,42(2):273-277.
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