【作者】 赵先恩； 朱树芸； 陈光； 和永瑞； 魏娜； 郑龙芳； 尤进茂；

【Author】 Xian-En Zhao;Shuyun Zhu;Guang Chen;Yongrui He;Na Wei;Longfang Zheng;Jinmao You;Shandong Provincial Key Laboratory of Life-Organic Analysis & Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University;

【机构】 曲阜师范大学化学与化工学院山东省生命有机分析重点实验室山东省绿色天然产物与医药中间体高校重点实验室；

【摘要】 化学衍生能够为色谱分离和质谱定性定量分析检测带来良好效果[1]。皂苷及其苷元类天然药物成分中的羟基类化合物因极性大、缺乏发色团和易于质谱离子化的基团,其色谱-质谱分析是具有挑战性的工作[2]。基于罗丹明分子中永久正电荷能够带来质谱增敏的特性,设计、合成一种具有显著质谱增敏效果的衍生化试剂:4’-羧基罗丹明(CRS),用于标记人参皂苷类、植物甾醇类等分析物中的活性游离羟基,衍生反应温和、快速、定量,联合串联分散液液微萃取技术,方法灵敏度高(pM~nM),基质干扰低,能满足血液、食品、药物中极微量羟基化合物的检测[3]。首次将商品化染色剂"丽思胺罗丹明B磺酰氯(LRSC)"用作衍生化试剂。通过衍生化标记6种帕金森病紧密相关的单胺类神经递质,与直接质谱检测相比,检出限降低2-3个数量级。采用活体大鼠脑微透析技术,将建立的分析方法应用于中药活性成分抗帕金森病活体药效学评价,结果良好,目前稿件在JCA二审中。更多还原

【Abstract】 Chemical derivatization can observably improve chromatographic separation and mass spectrometric(MS)analysis[1].It is a challenge to analyzing hydroxyl compounds,because they have large polarity,lack of chromophore and chemical structures of easy ionization[2].In this work,a new labeling reagent,4’-carboxy-substituted rosamine(CSR),which is highly reactive with hydroxyl group and has a permanent intramolecular positive charge,has been designed and synthesized for the derivatization of ginsengenins and phytosterols for the first time.The derivatization conditions were mild,rapid and quantitative.Combined with tandem dispersive liquid-liquid microextraction and UHPLC-MS/MS,the developed method was applied for the sensitive determination of hydroxyl analytes in plasma,food and medicine samples[3].Commercial lissamine rhodamine B sulfonyl chloride(LRSC) was used as derivatization reagent for the first time.The developed method was applied for the determination of monoamine neurotransmitters related with Parkinson’s disease(PD) by in vivo microdialysis sampling technique.更多还原