摘要
目的基于HPLC-Q-TOF-MS技术建立覆盆子的HPLC指纹图谱,并对化学成分进行快速鉴定。方法色谱分析采用Agilent Poroshell 120 EC-C 18色谱柱(4.6mm×50mm,2.7μm),流动相为甲醇:0.1%甲酸溶液(梯度洗脱),柱温30℃,流速为0.5mL·min^-1,检测波长254nm。以鞣花酸为参照峰,绘制10批不同产地覆盆子的HPLC图谱,使用《中药色谱指纹图谱相似度评价系统(2012版)》软件进行分析,确定共有峰。质谱分析采用电喷雾离子源(ESI)的飞行时间质谱(Q-TOF-MS),负离子模式采集数据,质荷比扫描范围为m/z 100~1000,用于共有峰的快速鉴定。结果建立了覆盆子的HPLC指纹图谱并标定了15个共有峰,相似度均大于0.93,通过高分辨Q-TO F-MS对共有峰进行了指认,鉴定了10个峰成分,分别为没食子酸、水杨酸、金丝桃苷、鞣花酸、紫云英苷、山柰酚-3-O-芸香糖苷、槲皮素、椴树苷、山奈酚、异鼠李素。结论该方法灵敏、简便、准确,建立的HPLC指纹图谱可用于覆盆子药材的质量评价。
OBJECTIVE To establish a new method base on HPLC-Q-TOF-MS for the fingerprint and the rapid identification of the components in Rubi Fructus.METHODS The chromatographic separation was performed on an Agilent Poroshell 120 EC-C 18 column(4.6mm×50mm,2.7μm).The mobile phase was consisited of methanol-0.1%formic acid by gradient elution at 30℃column temperature.The flow rate was 0.5mL·min^-1.The detection wavelength w as 254nm.With ellagic acid as the reference peak,10 batches of Rubus Chingii Hu from different origins were plotted by HPLC.The common peaks were determined by using the software of similarity evaluation system of chromatographic fingerp rint of traditional chinese medicine(2012 edition).Electro-spray ion(ESI)source and time-of-flight mass spectrometer(Q-TOF-MS)were used for the quali tative analysis in negative ion mode,the mass scan range was m/z 100-1000.RESULTS The HPLC fingerprint was set up with fifteen common peaks,the values were all greater than 0.93,and ten common peaks were identified by Q-TOF-MS as Gallic Acid,Salicylic Acid,Hyperoside,Ellagic Acid,Kaempfero l-3-O-glucoside,Kaempferol-3-O-rutinoside,Quercetin,Tiliroside,Kaempferol,Isorhamnetin.CONCLUSION The method was sensitive,simple,accurate,and suitable for the quality control of Rubus Chingii Hu.
作者
邓俊杰
DENG Jun-jie(Shaoxing Institute for Food and Drug Control,Shaoxing 312000,China)
出处
《海峡药学》
2020年第5期23-26,共4页
Strait Pharmaceutical Journal
