经典名方温经汤的基准样品特征图谱分析  

Analysis of Specific Chromatogram of Wenjingtang Reference Sample

作　　者：吴革林[1] 滕菲[2] 杨丹[2] 朱童 刘博男 张志杰[2] 杜玉苹 朱晶晶[2] WU Ge-lin;TENG Fei;YANG Dan;ZHU Tong;LIU Bo-nan;ZHANG Zhi-jie;DU Yu-ping;ZHU Jing-jing(Chinese Medicine Research Institute of Yangtze River Pharmaceutical Group Co.Ltd.,Taizhou 225321,China;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China)

机构地区：[1]扬子江药业集团有限公司中药研究院,江苏泰州225321 [2]中国中医科学院中药研究所,中药质量控制技术国家工程实验室,北京100700

出　　处：《中国实验方剂学杂志》2021年第22期7-14,共8页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家重点研发计划项目(2017YFC1701900,2018YFC1707002)。

摘　　要：目的:建立温经汤基准样品特征图谱。方法:采用高效液相色谱法(HPLC),建立温经汤基准样品的HPLC特征图谱分析方法,在此基础上,分别采用同一品牌多根色谱柱和4种不同品牌色谱柱,3个不同厂家仪器进行了系统适应性考察,计算相对保留时间,统计不同色谱柱、不同仪器的相对保留时间偏差,并对该方法进行方法学考察。采用超高效液相色谱-飞行时间质谱法(UPLC-Q-TOF-MSn)对温经汤基准样品成分进行鉴别,色谱条件为ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相乙腈(A)-0.1%甲酸水溶液(B)梯度洗脱(0~2.8 min,10%A;2.8~8.0 min,10%~18%A;8.0~12.2 min,18%~25%A;12.2~15.3 min,25%~40%A;15.3~17.4 min,40%A;17.4~20.5 min,40%~90%A),流速0.4 mL·min-1,柱温30℃。质谱条件为电喷雾离子源,正、负离子模式扫描,检测范围m/z 50~1600。结果:共选取了10个共有特征峰,通过对照品比对,指认了其中8个,分别为芍药苷(1号峰),芹糖甘草苷(2号峰),甘草苷(3号峰),阿魏酸(4号峰),甘草素(6号峰),桂皮醛(8号峰),丹皮酚(9号峰)和甘草酸(10号峰)。通过质谱分析,共鉴定了30个化合物,主要包括甘草三萜皂苷类和黄酮类、人参中人参皂苷类、白芍中单萜苷类和鞣质类、牛膝中甾酮类、当归中酚酸类成分。结论:所建立的温经汤特征图谱分析方法简便稳定、重复性好,通过质谱指认及来源归属,基本明确了温经汤基准样品的物质基础,可为后续温经汤的开发和质量控制提供参考依据。Objective:To control the quality of the reference sample of Wenjingtang by establishing the specific chromatograms. Method: On the basis of analyzing 15 batches of Wenjingtang freeze-dried powder samples, a high performance liquid chromatography(HPLC) specific chromatogram analysis method of Wenjingtang was established. The system adaptability was investigated and the retention time,relative retention value and deviation caused by different chromatographic columns and instruments were calculated by using the same brand of chromatographic columns,four different brands of chromatographic columns and instruments from three different manufacturers. The precision, repeatability and stability of this method was further completed. The possible chemical components of the freeze-dried powders were speculated and identified by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MSn).Chromatographic separation was performed on ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm)with acetonitrile(A)-0.1% formic acid aqueous solution(B)as mobile phase for gradient elution(0-2.8 min,10%A;2.8-8.0 min,10%-18%A;8.0-12.2 min,18%-25%A;12.2-15.3 min,25%-40%A;15.3-17.4 min,40%A;17.4-20.5 min,40%-90%A),and column temperature was set at 30 ℃ with flow rate of 0.4 mL·min-1.Mass spectrometry was performed on electrospray ionization,data were collected under positive and negative ion modes,and the detection range was m/z 50-1 600. Result: Ten characteristic peaks were selected as the distinguishing features in this specific chromatograms,and eight of them were identified by comparing with the reference standards,including paeoniflorin(peak 1),liquiritin apioside(peak 2),liquiritin(peak 3),ferulic acid(peak 4),iquiritigenin(peak 6),cinnamaldehyde(peak 8),paeonol(peak 9)and glycyrrhizic acid(peak10). By mass spectrometry analysis,30 compounds were identified,and the source of medicinal materials were assigned. It mainly contained triterpenoid saponins and flavonoids from Glycyrrhizae Radix et Rhi

关 键 词：经典名方 温经汤 基准样品 特征图谱 超高效液相色谱-飞行时间质谱法(UPLC-Q-TOF-MS^(n)) 相对保留时间 质量控制 

分 类 号：R22[医药卫生—中医基础理论] R28[医药卫生—中医学]