Ion-chromatographic Determination of Saccharides and Polyols in Tobacco with Separation by Matrix Solid Phase Dispersion
摘 要
采用基质固相分散法提取净化烟草中的糖和多元醇,并用离子色谱法进行测定.将烟草试样与石墨化炭黑球(质量比为1比4)充分研磨后装柱,用热水洗脱,洗脱液中的糖和多元醇用离子色谱测定.以CarboPac MA1阴离子色谱柱(4 mm×250 mm,5 μm)为固定相,用0.5 mol·L-1氢氧化钠溶液为流动相分离,用脉冲安培检测器检测.烟草试样中甘油、丙二醇、木糖醇、山梨醇、葡萄糖、果糖、蔗糖、麦芽糖和半乳糖9种成分在50 min内完全分离.方法的加标回收率在94.6%~105.3%之间,相对标准偏差(n=7)均小于3.0%.方法的检出限均小于50 μg·L-1.
Abstract
Saccharides and polyols in tobacco sample were separated by the method of matrix solid phase dispersion and determined by ion chromatography (IC).The sample was mixed with graphitized carbon black granules in the mass ratio of 1 to 4 and ground in a motar to make it a homogeneous dispersion.The dispersion was then filled into a solid phase extraction column.The SPE column was eluted with hot water to dissolve the saccharides and polyols from the sample in the dispersion.CarboPac MA1 (4 mm×250 mm,5 μm) anion exchange column was used as stationary phase,and 0.5 mol·L-1 sodium hydroxide solution was used as mobile phase.Conductivity detection was adopted.Nine components in tobacco,including glycero1,propylene glyco1,xylito1,sorbito1,fructose,glucose,sucrose,maltose and galactito1 were completely separated within 50 min.Values of detection limits (3S/N) found were all below 50 μg·L-1.Tests for recovery and precision were made,giving values of recovery ranged from 94.6%-105.3%,and of RSD′s (n=7) less than 3.0%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 云南省省院省校科技合作项目(2006YX17);中烟云南工业公司重大专项资助(2006Fl01)
收稿日期 2009/6/22
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备注叶艳青(1968-),女,云南昆明人,教授,从事分析化学教学研究工作.
引用该论文: YE Yan-qing,ZHANG Qun-fang,WU Na,YANG Guang-yu,HU Qiu-fen. Ion-chromatographic Determination of Saccharides and Polyols in Tobacco with Separation by Matrix Solid Phase Dispersion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(11): 1296~1299
叶艳青,张群芳,吴娜,杨光宇,胡秋芬. 基质固相分散-离子色谱法测定烟草中糖和多元醇[J]. 理化检验-化学分册, 2010, 46(11): 1296~1299
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【3】郑一新,朱晓兰.烟草中糖和尼古丁的自动分析[J].分析仪器,1995,15(3):28-30.
【4】马强,何友昭,肖协忠,等.烟草中糖的毛细管区带电泳分离[J].色谱,2002,20(3):230-232.
【5】毛多斌,曲志刚,张峻松,等.烟草中游离糖的毛细管气相色谱分析[J].色谱,2003,21(4):437.
【6】李忠,杨光宇,黄海涛,等.高效液相色谱测定烟草料液中的糖、甘油和丙二醇[J].分析化学,2002,30(6):687-689.
【7】SVOB T Z,FROBE Z,PEROVIC D.Analysis of selected alkaloids and sugars in tobacco extract[J].Journal of Chromatography A,1997,775(1):101-107.
【8】张龙翔,张庭芳,李令媛.生化实验方法技术[M].北京:高等教育出版社,1981:5-7.
【9】陈章玉,徐若飞,缪明明,等.高效液相色谱法测定烟草料液中几种保润成分[J].理化检验-化学分册,2006,42(10):1049-1051.
【10】唐坤甜,梁立娜,蔡亚岐,等.高效阴离子交换色谱分离-脉冲安培检测法测定烟草料液中的糖、糖醇和醇类化合物[J].分析化学,2007,35(9):1274-1278.
【11】BARKER S A.Matrix solid-phase dispersion[J].J Chromatogr A,2000,885(1):115-127.
【12】胡小钟,储小刚,余建新,等.基质固相分散和气相色谱-质谱法测定浓缩苹果汁中22种有机氯农药和15种拟除虫菊酯农药的残留量[J].分析测试学报,2004,23(5):38-42.
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