摘要
目的 建立消核糖浆的高效液相色谱(HPLC)指纹图谱,并测定其中10个有效成分的含量。方法 以12批消核糖浆为对象,采用超高效液相色谱-串联质谱(UPLC-MS/MS)法,以Athena C18(250 mm×4.6 mm,5μm)为色谱柱,以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,流速为1.0 mL/min,检测波长为210 nm。色谱图导入《中药色谱指纹图谱相似度评价系统(2012A版)》建立消核糖浆指纹图谱并进行相似度评价。采用ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.01%甲酸乙腈-0.01%甲酸水为流动相进行梯度洗脱,流速为0.4 mL/min,结合高分辨质谱仪,以电喷雾离子源进行正负离子扫描,测定12批消核糖浆中各主要成分的含量。结果 12批样品共标定33个共有峰,相似度均大于0.97;确认其中10个色谱峰,分别为王不留行黄酮苷、芍药苷、阿魏酸、柚皮苷、迷迭香酸、新橙皮苷、丹酚酸B、延胡索乙素、柴胡皂苷A、柴胡皂苷D;含量测定结果显示,上述10个成分在各自的质量浓度范围内线性关系良好(R 2>0.999),其含量分别为0.35~0.64、3.15~5.61、0.11~0.17、1.68~3.17、1.59~1.90、1.15~1.64、0.78~1.48、0.11~0.26、0.06~0.13、0.33~0.61 mg/mL。结论 12批消核糖浆的主要成分相似但含量有所差异;本研究建立的HPLC指纹图谱和UPLC-MS/MS含量测定方法可用于消核糖浆的全面质量评价。
OBJECTIVE To establish high performance liquid chromatography(HPLC) fingerprint of Xiaohe syrup and determine the contents of 10 effective ingredients in them.METHODS With 12 batches of Xiaohe syrup as samples,ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was adopted with Athena C18(250 mm×4.6 mm,5 μm) as the chromatographic column,acetonitrile-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution.The flow rate was 1.0 m L/min,and the detection wavelength was 210 nm.Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprint(2012A version) was imported to establish the fingerprint of Xiaohe syrup and evaluate the similarity.The content determination was performed on ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7 μm) chromatographic column,with 0.01% formic acid acetonitrile-0.01% formic acid water as mobile phase for gradient elution at a flow rate of 0.4mL/min;combined with high-resolution mass spectrometer,positive and negative ions were scanned with an electric spray ion source to determine the content of each main component in 12 batches of Xiaohe syrup.RESULTS A total of 33 common peaks were calibrated in 12 batches of samples,with similarities greater than 0.97;10 chromatographic peaks were confirmed,namely flavonoid glycosides,paeoniflorin,ferulic acid,naringin,rosmarinic acid,neohesperidin,salvianolic acid B,tetrahydropalmatine,saikosaponin A,and saikosaponin D.The results of content determination showed that the above 10 components had good linear relationships within their respective mass concentration ranges(all R 2>0.999),with contents ranging from 0.35 to 0.64,3.15 to 5.61,0.11 to 0.17,1.68 to 3.17,1.59 to 1.90,1.15 to 1.64,0.78 to 1.48,0.11 to 0.26,0.06 to 0.13,and 0.33 to 0.61 mg/mL,respectively.CONCLUSIONS The main components of 12 batches of Xiaohe syrup are similar,but the contents vary;HPLC fingerprint and UPLC-MS/MS content determination method established in this study can be used for comprehensive quality evaluation of Xiaohe syrup.
作者
李娜
汪潇潇
夏婕妤
刘宇
邓剑泠
陈万一
LI Na;WANG Xiaoxiao;XIA Jieyu;LIU Yu;DENG Jianling;CHEN Wanyi(Dept.of Pharmacy,Chongqing University Cancer Hospital,Chongqing 400030,China)
出处
《中国药房》
CAS
北大核心
2024年第12期1457-1462,共6页
China Pharmacy
基金
重庆市自然科学基金面上项目(No.cstc2020jcyjmsxmX0938)。
