六经头痛片HPLC指纹图谱建立及多指标成分定量测定研究  

Fingerprint and multi-components content simultaneous determination for Liujing Toutong Tablets by HPLC

作　　者：王月红[1] 游飞祥 王磊[3] 许浚[2,4] 袁雪海 龚苏晓[4] 朱晓丹[3] 韩彦琪[4] 张洪兵[4] 张铁军[4] 陈常青[4] WANG Yue-hong YOU Fei-xiang WANG Lei XU Jun YUAN Xue-hai GONG Su-xiao ZHU Xiao-dan HAN Yan-qi ZHANG Hong-bing ZHANG Tie-jun CHEN Chang-qing(Tianjin Medical University, Tianjin 300070, China Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China Tianjin Zhongxin Pharmaceutical Group Co., Ltd., Longshunrong Pharmaceutical Factory, Tianjin 300457, China Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China)

机构地区：[1]天津医科大学,天津300070 [2]天津中医药大学,天津300193 [3]天津中新药业集团股份有限公司隆顺榕制药厂,天津300457 [4]天津药物研究院,天津300193

出　　处：《中草药》2017年第20期4167-4173,共7页Chinese Traditional and Herbal Drugs

摘　　要：目的建立六经头痛片(LTT)HPLC指纹图谱,并采用波长切换技术同时定量测定3′-羟基葛根素、葛根素、大豆苷、特女贞苷和大豆苷元,为评价LTT质量提供依据。方法采用HPLC法,以Diamonsil C_(18)(250 mm×4.6 mm,5μm)为色谱柱,乙腈-0.1%磷酸水为流动相,分别建立LTT高极性和低极性部分指纹图谱,并采用波长切换技术同时测定LTT中3′-羟基葛根素、葛根素、大豆苷、特女贞苷和大豆苷元5种指标性成分量。结果分别建立了11批LTT高、低极性部分指纹图谱,其相似度均大于0.90;低极性指纹谱确定了16个共有峰,对其中12个共有峰进行了归属,11、12、13号峰来源于白芷,1、2、3、7号峰来源于葛根,8号峰来源于女贞子,5、6号峰来源于川芎,15号峰来源于藁本,4号峰为川芎和藁本的共有峰,对其中7个共有峰经对照品指认,分别为葛根素(1号峰)、3′-甲氧基葛根素(2号峰)、大豆苷(3号峰)、阿魏酸(4号峰)、大豆苷元(7号峰)、欧前胡素(11号峰)和异欧前胡素(13号峰);高极性指纹图谱确定了10个共有峰,其中2~9号峰来源于葛根,1、10号峰来源于女贞子,对其中5个共有峰经对照品指认,分别为3′-羟基葛根素(2号峰)、葛根素(3号峰)、3′-甲氧基葛根素(4号峰)、大豆苷(7号峰)和特女贞苷(10号峰)。多成分定量测定中,3′-羟基葛根素在71.60~716.00 ng(r=0.999 1)、葛根素在407.78~4 077.80 ng(r=0.999 4)、大豆苷在90.72~907.20 ng(r=0.999 9)、特女贞苷在95.80~958.00 ng(r=0.999 1)、大豆苷元在21.98~219.80 ng(r=0.999 9)线性关系良好,平均加样回收率和相应的RSD分别为101.1%、1.38%,97.8%、0.72%,99.1%、0.75%,97.8%、2.75%,98.7%、0.70%;10批样品中3′-羟基葛根素量为3.08~3.84 mg/m L、葛根素17.71~21.24 mg/m L、大豆苷3.51~4.71 mg/m L、特女贞苷1.40~5.69 mg/m L、大豆苷元0.66~0.86 mg/m L。结论该法稳定可靠、重复性好,通过HPLC指纹图谱结合多指标定量测定方法较全面地反�Objective To establish the HPLC fingerprint of Liujing Toutong Tablets（LTT） and multi-wavelength method for determination of the contents of 3′-hydroxy puerarin, puerarin, daidzin, nuezhenide, and daidzein, so as to provide a reference for the quality control. Methods Using the method of HPLC, the fingerprint chromatography of high polarity and low polarity were established, with a mobile phase of acetonitrile-0.1% phosphoric acid and Diamonsil C_（18） column（250 mm × 4.6 mm, 5 μm）. Furtherly, the Diamonsil C18 column was used with a mobile phase of acetonitrile-0.1% acetic acid gradient elution to determine the five contents. Results The fingerprint chromatography of high and low polarities with 11 batches of LTT were established, and the similarities of 11 batches were all over 0.90. The low polarity fingerprint chromatography included 16 mutual peaks, 12 of which belonged to herbs： No. 11, 12, 13 belonged to Angelicae Dahuricae Radix, No. 1, 2, 3, 7 belonged to Puerariae Lobatae Radix, No. 8 belonged to Ligustri Lucidi Fructus, No. 5, 6 belonged to Chuanxiong Rhizoma, No. 15 belonged to Ligustici Rhizoma et Radix and No. 4 belonged to Chuanxiong Rhizoma and Ligustici Rhizoma et Radix. Seven peaks including puerarin（No. 1）, 3′-methoxy puerarin（No. 2）, daidzin（No. 3）, ferulic acid（No. 4）, daidzein（No. 7）, imperatorin（No. 11）, and isoimperatorin（No. 13） were verified by standard compounds. The high polarity fingerprint chromatography included 10 mutual peaks, among them No. 2—9 belonged to Puerariae Lobatae Radix, No. 1, 10 belonged to Ligustri Lucidi Fructus. Five peaks including 3′-hydoxypuerarin（No. 2）, puerarin（No. 3）, 3′-methoxypuerarin（No. 4）, daidzin（No. 7） and specnuezhenide（No. 10） were verified by standard compounds. The five active components were well separated and showed good lineaeity, such as 3′-hydroxy puerarin 71.60—716.00 ng（r = 0.999 1）, puerarin 407.78—4 077.80 ng（r = 0.999 4）, daidzin 90.72—907.20 ng（r

关 键 词：六经头痛片 HPLC 指纹图谱 3′-羟基葛根素 葛根素 大豆苷 特女贞苷 大豆苷元 白芷 葛根 女贞子 川芎 藁本 

分 类 号：R286.02[医药卫生—中药学]