三棱UPLC-UV特征图谱研究  

UPLC-UV Characteristic Fingerprint of Sparganii Rhizoma

作　　者：唐嵩媛 赵琦琦 孙晖[1] 闫广利[1] 王喜军[1] 车延柠 张秀玲 TANG Song-yuan;ZHAO Qi-qi;SUN Hui;YAN Guang-li;WANG Xi-jun;CHE Yan-ning;ZHANG Xiu-ling(Heilongjiang University of Chinese Medicine,Engineering Research Center of Efficiency Evaluation and Industrialization Development of Classical Prescriptions,Ministry of Education,Research Center of Chinmedomics,National Administration of Traditional Chinese Medicine,Harbin 150040,China;Harbin No.4 Chinese Medicine Factory Co.,Ltd.,Harbin 150500,China)

机构地区：[1]黑龙江中医药大学/教育部经典名方有效性评价及产业化开发工程研究中心/国家中医药管理局中医方证代谢组学研究中心,黑龙江哈尔滨150040 [2]哈尔滨中药四厂有限公司,黑龙江哈尔滨150500

出　　处：《中国现代中药》2022年第6期1009-1017,共9页Modern Chinese Medicine

基　　金：黑龙江省应用技术研究与开发计划重大项目(GA18C004);黑龙江中医药大学科研基金项目(2018xy01)。

摘　　要：目的:建立三棱化学成分的超高效液相色谱-紫外法(UPLC-UV)特征图谱,并对主要特征峰进行指认。方法:色谱柱为Waters ACQUITY UPLC HSS T3柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-0.1%磷酸水溶液,线性梯度洗脱,双波长切换检测,0~12 min为300 nm,12~16 min为240 nm,测定10批三棱药材UPLCUV图,确定共有特征峰并计算相似度,利用对照品及超高效液相色谱-四极杆飞行时间质谱法(UPLC-Q/TOF-MS)对主要特征峰进行指认。结果:采集了10批三棱药材UPLC-UV指纹图谱,确定11个特征峰,相似度均大于0.9,认定了9个特征峰,其中通过对照品指认了咖啡酸、对羟基苯甲酸、对香豆酸,通过质谱解析指认了2个苯丙素乙酰蔗糖酯、3个苯丙素甘油酯及首次在三棱中发现的三棱酮。结论:建立了三棱UPLC-UV特征图谱,能够表征不同结构类型的三棱化学成分,为三棱药材质量控制提供了参考。Objective:To establish the UPLC-UV characteristic fingerprint for Sparganii Rhizoma and identify the main peaks.Methods:The UPLC conditions are as follows:Waters ACQUITY UPLC HSS T3 column(100 mm × 2.1 mm,1.8 μm),mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution,linear gradient elution,and detection at 300nm in 0-12 min and 240 nm in12-16 min.The chromatograms of 10 batches of Sparganii Rhizoma were determined to screen the common peaks and calculate their similarities.The characteristic peaks were characterized by UPLC-Q/TOF-MS and the reference standards.Results:The UPLC-UV chromatograms of10 batches of Sparganii Rhizoma showed 11 common peaks,with similarities>0.9.A total of 9 compounds were identified,with caffeic acid,p-hydroxybenzoic acid,and p-coumaric acid by comparison with the reference standards,and 2 phenylpropanoid acetyl sucrose esters,3 phenylpropanoid glycerols,and sanalengone(discovered for the first time in Sparganii Rhizoma) by MS.Conclusion:The UPLC-UV characteristic fingerprint of Sparganii Rhizoma was established,which can characterize more structure types of chemical components in Sparganii Rhizoma,and thus it is applicable to the quality control of Sparganii Rhizoma.

关 键 词：三棱 超高效液相色谱-紫外法特征图谱 苯丙素乙酰蔗糖酯 苯丙素甘油酯 三棱酮 

分 类 号：R284[医药卫生—中药学]