中国中药杂志

2018, v.43(22) 4469-4473

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柱前衍生化UPLC-MS/MS测定12种单糖含量的方法学研究及其应用
Analysis of monosaccharide composition of twelve polysaccharides by pre-column derivatization procedure UPLC-MS/MS

梁宇庭;周骏辉;南铁贵;钱丹;宋瑞琦;赵雅秋;袁媛;
LIANG Yu-ting;ZHOU Jun-hui;NAN Tie-gui;QIAN Dan;SONG Rui-qi;ZHAO Ya-qiu;YUAN Yuan;School of Chinese Materia Medica,Capital Medical University;National Resource Center for Chinese Materia Medica,China Academy of Chinese Medical Sciences;School of Traditional Chinese Medicine,Guangdong Pharmaceutical University;

摘要(Abstract):

建立了1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化UPLC-MS/MS检测12种单糖的方法,同时对蜜环菌中多糖的单糖组成成分进行了分析。安捷伦ZORBAX RRHD Eclipse Plus C18分析柱(2. 1 mm×100 mm,1. 8μm),95%乙腈(A)和乙酸铵-5%乙腈-水(B)为流动相梯度洗脱,质谱为电喷雾离子源(ESI)接口,采用负离子多反应监测模式(MRM)进行检测。结果表明,基于UPLC-MS/MS所建立的单糖检测方法,12种单糖成分在各自线性范围内线性关系良好(R2> 0. 990),加样回收率为92. 30%~105. 6%。在蜜环菌样品中,可检测出除阿洛糖外的11种单糖组分。该试验所建立的方法稳健,重复性和准确度高,适用于蜜环菌等的单糖成分的含量测定。
This study is to establish a pre-column derivatization procedure with 1-phenyl-3-methyl-5-pyrazolone(PMP) UPLC-MS/MS method for the determination of the monosaccharide composition of 12 polysaccharides. At the same time,the monosaccharide components of polysaccharides in Armillaria gallica were analyzed. The separation was performed on a ACQUITY ZORBAX RRHD Eclipse Plus C18 column(2. 1 mm × 100 mm,1. 8 μm),using 95% acetonitrile(A) and ammonium acetate-5% acetonitrile-water(B) as mobile phase with gradient elution. The target components were detected in multiple-reaction monitoring(MRM) mode by mass spectrometry with electrospray ionization(ESI) source operated in ionization mode. The results showed that based on the monosaccharides detection method established by UPLC-MS/MS,the linearity of the 12 monosaccharides components were linear in their linear range(R2> 0. 990),and the recovery rate were 92. 30%-105. 6%. 11 monosaccharides such as fructose,mannose,and glucose were detected in A. gallica samples. The method established in this experiment is robust,highly reproducible and accurate,and is suitable for the determination of monosaccharide components such as A. gallica.

关键词(KeyWords): UPLC-MS/MS;PMP衍生化;单糖组成;蜜环菌
UPLC-MS/MS;PMP derivatization;monosaccharide composition;Armillaria gallica

Abstract:

Keywords:

基金项目(Foundation): 中央级公益性科研院所基本科研业务费专项(ZZ10-008);; 中央本部级重大支减项目(2060302)

作者(Author): 梁宇庭;周骏辉;南铁贵;钱丹;宋瑞琦;赵雅秋;袁媛;
LIANG Yu-ting;ZHOU Jun-hui;NAN Tie-gui;QIAN Dan;SONG Rui-qi;ZHAO Ya-qiu;YUAN Yuan;School of Chinese Materia Medica,Capital Medical University;National Resource Center for Chinese Materia Medica,China Academy of Chinese Medical Sciences;School of Traditional Chinese Medicine,Guangdong Pharmaceutical University;

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DOI: 10.19540/j.cnki.cjcmm.20180724.004

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