摘要
采用超高效液相色谱-四极杆-飞行时间质谱联用技术(UPLC-Q-TOF-MS/MS)快速鉴别香青兰的化学成分,并对其主要成分进行UPLC含量测定。质谱分析采用电喷雾离子源(ESI),负离子模式下采集数据,结合对照品的保留时间和质谱信息、自建化合物数据库、PubChem数据库等,从香青兰中鉴定化合物68个,其中黄酮类36个、苯丙素类22个,苯酚类4个、其他类化合物6个。在此基础上,建立同步测定木犀草素-7-O-葡萄糖醛酸苷、芹菜素-7-O-葡萄糖醛酸苷、迷迭香酸、香叶木素-7-O-葡萄糖醛酸苷、田蓟苷、金合欢素-7-O-葡萄糖醛酸苷、金合欢素-7-O-(6″-O-丙二酸单酰)-葡萄糖苷和金合欢素等8种主要成分的UPLC定量方法。采用Waters ACQUITY BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),以乙腈-含0.1%甲酸和0.1%磷酸的水溶液为流动相进行梯度洗脱,检测波长330 nm,流速0.4 mL·min^(-1),柱温35℃。上述8种成分在较宽的质量浓度范围(50或100倍)内,呈现良好的线性关系(r≥0.9999),平均回收率为97.5%~105.1%,RSD为0.90%~3.4%(n=6),该法简便、准确、可靠。17批香青兰样品中,上述8种成分的质量分数分别为0.405~2.10、0.063~0.342、0.446~2.43、0.415~1.47、1.57~4.34、0.173~0.386、1.00~5.40、0.069~0.207 mg·g^(-1),说明其内在质量存在较大差异,需进行良好的质量控制以保障其药效。该研究为香青兰的药效物质快速发现、整体质量控制与评价以及质量标准的制修订提供科学依据。
Ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS/MS)was used to rapidly identify the chemical components in Dracocephalum moldavica L.,and the main components were determined by UPLC.MS analysis was conducted with electrospray ionization(ESI)in negative mode.The chemical components were identified by comparison with the retention time and mass spectra of reference compound s,selfbuilt database,PubChem database,etc.A total of 68 compounds were identified from D.moldavica L.,including 36 flavonoids,22 phenylpropanoids,4 phenols and 6 others.On this basis,an UPLC quantitative method was established to simultaneously determine 8 main components, including luteolin-7-O-glucuronide, apigenin-7-O-glucuronide, rosmarinicacid, diosmetin-7-O-glucuronide, tilianin, acacetin-7-O-glucuronide, acacetin-7-O-(6''-O-malonyl)-glucoside and acacetin.The quantitative analysis was performed on Waters ACQUITY BEH C18 column (2.1 mm× 100 mm, 1.7 μm) with mobilephase of acetonitrile- aqueous solution containing 0.1% formic acid and 0.1% phosphoric acid for gradient elution,thedetection wavelength of 330 nm, the flow rate of 0.4 mL·min^(-1), and the column temperature of 35 ℃. The above 8components showed good linearity (r≥ 0.999 9) in a wide mass concentration range (50 or 100 times). The average recoverieswere 97.5%~105.1%, and the relative standard deviations (RSDs) were 0.90%~3.4% (n = 6). The present method was simple,accurate and reliable. The content ranges of the above 8 components in 17 batches of D. moldavica L. were 0.405~2.10,0.063~0.342, 0.446~2.43, 0.415~1.47, 1.57~4.34, 0.173~0.386, 1.00~5.40, and 0.069~0.207 mg·g^(-1), respectively, indicatingthat there were great differences in their internal quality, and good quality control was required to ensure thepharmacodynamics. This study provides a scientific basis for the rapid discovery of pharmacodynamic substances, the whol equality control, and the formulation or revision of quality standards in D. moldavica L.
作者
胥明磊
高慧敏
张永欣
李治建
丁阳
王清荣
霍仕霞
冯伟红
康雨彤
陈两绵
王智民
XU Ming-lei;GAO Hui-min;ZHANG Yong-xin;LI Zhi-jian;DING Yang;WANG Qing-rong;HUO Shi-xia;FENGWei-hong;KANG Yu-tong;CHEN Liang-mian;WANG Zhi-min(Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Uygur Medical Hospital of Xinjiang Uygur Autonomous Region,Urumqi 830049,China;Xinjiang Key Laboratory of Evidence-Based and Translation,Hospital Preparation of Traditional Chinese Medicine,Urumqi 830049,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2024年第23期6352-6367,共16页
China Journal of Chinese Materia Medica
基金
中央引导地方科技发展专项(ZYYD2023C10)
“天山创新团队计划”项目(2024D14018)
中国中医科学院基本科研业务费自主选题项目(ZXKT22027)。
关键词
香青兰
超高效液相色谱-四极杆-飞行时间质谱联用技术
定性分析
含量测定
质量控制
Dracocephalum moldavica L.
ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS)
qualitative analysis
content determination
quality control
