目的:分析化橘红中的主要化学成分,并比较这些化学成分在毛橘红与光橘红中组成和含量的异同。方法:采用HPLC-DAD-MS/MS对化橘红中一些主要化学成分进行定性研究。色谱柱为Dikma Diamasil C18柱(4.6 mm×250 mm,5μm),流动相为0.5%甲酸水-甲醇,流速为350μL.min-1,进样量为10μL。质谱的离子源为电喷雾离子源,采用了正负离子模式两种扫描方式。结果:通过样品、对照品及文献中相应成分的质谱数据、紫外光谱信息归属了柚皮苷、野漆树苷等13个化合物,毛橘红中柚皮苷、野漆树苷、水合氧化前胡素和异欧前胡素的含量均明显高于光橘红。结论:HPLC-DAD-MS/MS分析可以获得黄酮类及香豆素类化学物丰富的结构信息,为化橘红化学成分的定性提供了一种快速有效的方法,也为化橘红药材的质量控制提供更多科学依据。

The study is aimed to analyze components in Exocarpium citri grandis from Citrus grandis′ Tomentosa′ and Citrus grandis(L.) Osbeck.HPLC-DAD-MS/MS was used to identify main components in citri grandis Exocarpium.The MS fragmentation regularity of flavonoid and coumarins were proposed.The mobile phase of HPLC was consisted of 0.5% formic acid in water and methanol.The analytical column was Dikma Diamonsil C18(4.6 mm×250 mm,5 μm).The flow rate was 350 μL·min-1.And the injection volume was 10 μL.The ionization source was ESI in positive or negative ion mode.The result showed that naringin,rhoifolin and eleven other components were tentatively identified in chromatograms based on their retention time,reference standards,MS data and UV spectra comparison in published papers.The content of naringin,rhoifolin,oxypeucedanin hydrate and isoimperatorin in citri grandis Exocarpium from Citrus grandis′ Tomentosa′ were higher than those in citri grandis Exocarpium from Citrus grandis(L.) Osbeck.It is concluded that the structural information was obtained through HPLC-DAD-MS/MS.It provides an accurate and fast method to identify components in citri grandis Exocarpium.More scientific information has been provided for quality control of citri grandis Exocarpium.

广东省科技厅广东省部产学研项目(2010B090400533):中药化学对照品制备关键技术及商业化运营平台的构建,负责人:徐新军;科学技术部国际科技合作项目(2009DFA31230):基于澳洲TGA药材注册的南药质量评价体系研究,主持人:杨得坡