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引用本文:刘敏,张晓芹,黄绳武,余乐,范蕾,陈梦,陈张金,陈桂云,陈琴鸣,顾正兵.畲药树参茎化学成分分析及抗炎活性部位高效液相指纹图谱的建立[J].中国现代应用药学,2022,39(19):2505-2510.
LIU Min,ZHANG Xiaoqin,HUNG Shengwu,YU Le,FAN Lei,CHEN Meng,CHEN Zhangjin,CHEN Guiyun,CHEN Qinming,GU Zhengbing.Analysis Chemical Constituents in the Stems of She Medicine Dendropanax Dentiger and Establishing HPLC Fingerprint of Its Anti-inflammatory Active Fraction[J].Chin J Mod Appl Pharm(中国现代应用药学),2022,39(19):2505-2510.
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畲药树参茎化学成分分析及抗炎活性部位高效液相指纹图谱的建立
刘敏1, 张晓芹2, 黄绳武3, 余乐1, 范蕾1, 陈梦1, 陈张金1, 陈桂云1, 陈琴鸣1, 顾正兵4
1.丽水市质量检验检测研究院, 浙江 丽水 323000;2.丽水市中医院, 浙江 丽水 323000;3.浙江中医药大学, 杭州 310053;4.泰州丹鼎生物科技有限公司, 江苏 泰州 225400
摘要:
目的 对畲药树参茎所含化学成分进行确证分析,并建立抗炎活性部位的高效液相色谱指纹图谱。方法 采用液相色谱-质谱联用、核磁共振波谱仪等分析仪器分离鉴定树参茎中的化学成分;采用高效液相色谱法建立抗炎活性部位指纹图谱:色谱柱为Waters SunfireTM C18(4.6 mm×250 mm,5 μm),流动相为乙腈-混合水溶液(含甲酸0.2%和四氢呋喃0.2%),梯度洗脱。检测波长为256 nm,柱温30 ℃,体积流量为1.0 mL·mim–1,分析时间为80 min,进样量为5 μL。结果 从树参茎中共分离鉴定出10个化合物,分别是绿原酸(1)、3,4-O-二咖啡酰基奎宁酸(2)、3,5-O-二咖啡酰基奎宁酸(3)、4,5-O-二咖啡酰基奎宁酸(4)、saikolignanoside A(5)、芦丁(6)、山柰酚-3-O-芸香糖苷(7)、紫丁香苷(8)、松柏醇(9)、芥子醛葡萄糖苷(10);12批样品抗炎活性部位指纹图谱相似度为0.901~0.992,均符合要求。结论 树参茎中主要含有酚酸类、黄酮类、苯丙素类化合物;建立的指纹图谱不仅能体现树参茎抗炎的化学物质基础,而且鉴别方法简便、重复性好,可为树参茎的品质评价及主要抗炎活性成分的确证提供科学依据。
关键词:  树参茎  抗炎  活性部位  高效液相色谱法  指纹图谱
DOI:10.13748/j.cnki.issn1007-7693.2022.19.011
分类号:R284.1
基金项目:浙江省药品监督管理局科技计划项目(2020003)
Analysis Chemical Constituents in the Stems of She Medicine Dendropanax Dentiger and Establishing HPLC Fingerprint of Its Anti-inflammatory Active Fraction
LIU Min1, ZHANG Xiaoqin2, HUNG Shengwu3, YU Le1, FAN Lei1, CHEN Meng1, CHEN Zhangjin1, CHEN Guiyun1, CHEN Qinming1, GU Zhengbing4
1.Lishui Institute for Quality Inspection and Testing, Lishui 323000, China;2.Lishui Hospital of Traditional Chinese Medicine, Lishui 323000, China;3.Zhejiang Chinese Medical University, Hangzhou 310053, China;4.Taizhou Danding Biotechnology Co., Ltd., Taizhou 225400, China
Abstract:
OBJECTIVE To confirm and analyze the chemical constituents in the stems of Dendropanax dentiger,and establish the HPLC fingerprint of its anti-inflammatory active fraction. METHODS Compounds were isolated and identified by LC-MS,NMR and other analysis instruments.HPLC with Waters SunfireTM C18 column (4.6 mm×250 mm,5 μm) was used.Mobile phase consisted acetonitrile-aqueous solution including 0.2% formic acid and 0.2% tetrahydrofuran with gradient elution.Detection wavelength was 256 nm.Column temperature was 30℃.Flow rate was 1.0 mL·mim–1 and analytic time was 80 min.Injection volume was 5 μL.RESULTS Ten compounds were isolated and identified as chlorogenic acid (1),3,4-O-caffeoylquinic acid methyl ester (2),3,5-O-caffeoylquinic acid methyl ester (3),4,5-O-caffeoylquinic acid methyl ester (4),saikolignanoside A (5),rutin (6),kaempferol-3-O-rutinoside (7),syringin (8),coniferol (9),sinapaldehyde glucoside (10).Under the same fingerprint chromatogram condition,the methodological results were satisfactory to 12 batches of the anti-inflammatory active fractions.And the similarity range was 0.901-0.992.CONCLUSION The stems of Dendropanax dentiger mainly contain phenolic acids,flavonoids and phenylpropanoids.The established fingerprint can not only reflect the chemical basis of anti-inflammatory of the She medicine,but the identification method also is simple and reproducible.It can provide a scientific basis for the quality evaluation and the confirmation of main anti-inflammatory active components of the stems of Dendropanax dentiger.
Key words:  stems of Dendropanax dentiger  anti-inflammatory  active fraction  HPLC  fingerprint
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