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柱前衍生超高效液相色谱-串联四极杆质谱法测定仙草多糖组成及其含量
  • ISSN号:1004-4957
  • 期刊名称:分析测试学报
  • 时间:2013.2.25
  • 页码:143-149
  • 分类:O657.63[理学—分析化学;理学—化学] Q53[生物学—生物化学]
  • 作者机构:[1]华东理工大学化学与分子工程学院,上海200237
  • 相关基金:国家青年科学基金资助项目(21105027)
  • 相关项目:双酶孔径梯度杂化整体蛋白质在线酶反应器研究
中文摘要:

建立了测定仙草多糖组成及其含量的超高效液相色谱-串联四极杆质谱分析方法。仙草样品在碱性条件下用沸水提取,提取液经固相萃取小柱净化后加三氟乙酸在110℃水解,然后采用1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生。以WatersACQUITYUPLCBEHC18(2.1mmi.d.×50mm,1.7μm)为分析柱,乙腈和缓冲盐溶液(0.5mmol/L乙酸铵-0.05%乙酸)为流动相进行梯度洗脱分离,流速0.5mL/min,电喷雾正离子多反应监测模式检测,内标法定量。结果显示8种单糖在1~100μmol/L浓度范围内呈良好的线性关系,相关系数r2均大于0.96,方法的回收率为84%-112%,相对标准偏差(RSD)不高于4.7%。仙草多糖由甘露糖、鼠李糖、核糖、葡萄糖醛酸、半乳糖醛酸、葡萄糖、半乳糖和木糖8种单糖组成,其摩尔百分比为7.4%、5.7%、4.2%、0.9%、28.4%、26.5%、16.4%和10.6%。该法简单、快速、灵敏高、重现性好,可用于仙草多糖的单糖组成分析和含量测定。

英文摘要:

An ultra-high performance liquid chromatography- tandem quadrupole mass spectrometric method was developed for the determination of monosaccharide composition and content in Mesona Chinensis Benth polysaccharides. Mesona Chinensis Benth Polysaccharides were extracted with hot water under alkaline environment, cleaned with Cls SPE cartridge, and then hydrolysised with triflu- oroacetic acid at 110 ~C. The monosaccharaides were derivated with 1-phenyl-3-methyl-5-pyrazolone (PMP) , and separated at a flow rate of 0. 5 mL/min on a Waters ACQUITY UPLC BEH Cls column (2. 1 mm i. d. x50 mm, 1.7 I~m) at 35 ~C, by using acetonitrile and 0. 5 mmol/L ammonium ace- tate -0. 05% acetic acid buffer as mobile phase by a gradient elution. The analysis of target com- pounds was performed in multiple reaction monitoring (MRM) mode via positive electrospray ioniza- tion, and quantified by the internal standard method. The developed method showed good linearities over the concentration range of 1 - 100 μmol/L for all monosaccharaides with correlation coefficient (r2) more than 0. 96. The spiked recoveries were between 84% and 112% , and the relative stand- ard deviations (RSD) were no more than 4.7%. The results showed that Mesona Chinensis Benth polysaccharides consisted of eight monosaccharides, including mannose, rhamnose, ribose, glucu- ronic acid, galacturonic acid, glucose, galactose, xylose, with the molar percentages of 7.4% ,5.7%, 4. 2%, 0.9%, 28.4%, 26. 5%, 16.4% and 10. 6%, ple, rapid, sensitive and convenient, and could be applied in Benth polysaeeharides. respectively. The method is simthe analysis of Mesona Chinensis Benth polysaccharides.

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期刊信息
  • 《分析测试学报》
  • 北大核心期刊(2011版)
  • 主管单位:广东省科学技术厅
  • 主办单位:中国分析测试协会 中国广州分析测试中心
  • 主编:陈小明
  • 地址:广州市先烈中路100号34栋B201中国广州分析测试中心内
  • 邮编:510070
  • 邮箱:fxcsxb@china.com
  • 电话:020- 37656606
  • 国际标准刊号:ISSN:1004-4957
  • 国内统一刊号:ISSN:44-1318/TH
  • 邮发代号:46-104
  • 获奖情况:
  • 获广东省第一、二届优秀期刊奖
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:25362