川芎饮片标准汤剂的HPLC及物理指纹图谱研究
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摘要
目的制备15批川芎饮片标准汤剂,建立其HPLC指纹图谱和物理指纹图谱并对其进行质量评价。方法按《中药配方颗粒质量控制与标准制定技术要求(征求意见稿)》中标准汤剂制备条件,制备15批川芎饮片标准汤剂,采用HPLC,流动相为0.6%磷酸水溶液-乙腈,进行梯度洗脱,柱温30℃,体积流量1.0 mL/min,检测波长324 nm,建立川芎饮片标准汤剂的HPLC指纹图谱;并建立由9个2级指标(相对均齐度指数、颗粒间空隙率、卡尔指数、松密度、振实密度、干燥失重、吸湿性、豪斯纳比、休止角)构成的物理指纹图谱。结果 HPLC对照指纹图谱中主要共有峰有13个,确认3个,分别为绿原酸、咖啡酸和阿魏酸。以阿魏酸为参照峰,分析了各共有峰的相对保留时间和相对峰面积,并规定了各共有峰相对保留时间和相对峰面积的限度。建立了HPLC及物理指纹图谱,并规定其相似度均不应低于0.9。结论建立的川芎饮片标准汤剂的HPLC和物理指纹图谱可作为合理稳定的质量评价指标,为川芎配方颗粒的研制及质量控制提供参考。
Objective To prepare 15 batches of Chuanxiong Rhizoma standard decoction,and establish HPLC fingerprint and physical fingerprint for quality evaluation.Methods Fifteen batches of Chuanxiong Rhizoma standard decoction were prepared according to preparation conditions of the traditional Chinese medicine(TCM) standard decoction in "Technical Requirements for Quality Control and Standard Formulation of Prescription Granules of TCM(draft for soliciting opinions)".The mobile phase of HPLC consisted of 0.6% aqueous solution of phosphoric acid and acetonitrile with gradient elution,column temperature of that was 30 ℃,flow rate of that was 1.0 mL/min and detection wavelength of that was 324 nm.Physical fingerprint that consisted of nine secondary indexes(relative homogeneity index,intergranular porosity,Karl index,loose density,vibrating density,dry weight loss,hygroscopicity,Hausner ratio,and angle of repose) was established.Results There were 13 common peaks in the HPLC control fingerprint,and three of them were identified as chlorogenic acid,caffeic acid,and ferulic acid respectively.Taking ferulic acid as a reference peak,the relative retention time and relative peak area of each co-owned peak were analyzed,and the limits of relative retention time and relative peak area of each co-owned peak were specified.The HPLC and physical fingerprint were established,and the similarity should greater than 0.9.Conclusion The HPLC and physical fingerprint of the Chuanxiong Rhizoma standard decoction can be used as reasonable and stable index to evaluate the quality of Chuanxiong Rhizoma standard decoction.Which provides a reference for the preparation and quality control of Chuanxiong Rhizoma dispensing granule.
Objective To prepare 15 batches of Chuanxiong Rhizoma standard decoction,and establish HPLC fingerprint and physical fingerprint for quality evaluation.Methods Fifteen batches of Chuanxiong Rhizoma standard decoction were prepared according to preparation conditions of the traditional Chinese medicine(TCM) standard decoction in "Technical Requirements for Quality Control and Standard Formulation of Prescription Granules of TCM(draft for soliciting opinions)".The mobile phase of HPLC consisted of 0.6% aqueous solution of phosphoric acid and acetonitrile with gradient elution,column temperature of that was 30 ℃,flow rate of that was 1.0 mL/min and detection wavelength of that was 324 nm.Physical fingerprint that consisted of nine secondary indexes(relative homogeneity index,intergranular porosity,Karl index,loose density,vibrating density,dry weight loss,hygroscopicity,Hausner ratio,and angle of repose) was established.Results There were 13 common peaks in the HPLC control fingerprint,and three of them were identified as chlorogenic acid,caffeic acid,and ferulic acid respectively.Taking ferulic acid as a reference peak,the relative retention time and relative peak area of each co-owned peak were analyzed,and the limits of relative retention time and relative peak area of each co-owned peak were specified.The HPLC and physical fingerprint were established,and the similarity should greater than 0.9.Conclusion The HPLC and physical fingerprint of the Chuanxiong Rhizoma standard decoction can be used as reasonable and stable index to evaluate the quality of Chuanxiong Rhizoma standard decoction.Which provides a reference for the preparation and quality control of Chuanxiong Rhizoma dispensing granule.
引文
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[19]李鹏程,刘涛,张文文,等.基于Qb D理念的黄槐片制备工艺及物理指纹图谱研究[J].中草药,2018,49(7):1576-1582.
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[23]李远辉,伍振峰,李延年,等.基于粉体学性质分析浸膏干燥工艺与中药配方颗粒制粒质量的相关性[J].中草药,2017,48(10):1930-1935.
[24]徐玉玲,谢敏,梁悦,等.基于Qb D理念优选川明参口含片的制备工艺[J].中国实验方剂学杂志,2018,24(17):1-6.
[25]仝家羽,赵嵘,代云桃,等.当归标准汤剂质量评价体系的建立[J].中国实验方剂学杂志,2017,23(7):18-23.
[26]方雯雯,成守玲,陈培胜,等.白芷药材-饮片-提取物及配方颗粒的HPLC特征图谱相关性研究[J].中草药,2016,47(18):3211-3214.
[27]杨胤,冯怡,徐德生,等.干燥工艺与中药提取物物理性质的相关性研究[J].中国药学杂志,2008,43(17):1295-1299.
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[2]郑春松,徐筱杰,叶蕻芝,等.川芎活血化瘀和行气止痛作用的计算机模拟研究[J].中华中医药杂志,2015,30(5):1432-1436.
[3]高兵.川芎鉴定及临床应用价值分析[J].中国实用医药,2017,12(31):131-132.
[4]姜溪,邵凤,郑歆,等.川芎救心滴丸对动物实验性心肌缺血的保护作用研究[J].现代药物与临床,2014,29(5):476-480.
[5]金玉青,洪远林,李建蕊,等.川芎的化学成分及药理作用研究进展[J].中药与临床,2013,4(3):44-48.
[6]徐育新.川芎鉴定及临床应用分析[J].微量元素与健康研究,2016,33(3):36-37.
[7]郑怡然,韦玮,杨秀伟.川芎中抑制脂多糖诱导的RAW264.7和BV2细胞系NO生成的新的丁苯酞衍生物-川芎螺内酯[J].中草药,2018,49(7):1497-1503.
[8]韩炜.川芎的化学成分与药理作用研究进展[J].中国现代中药,2017,19(9):1341-1349.
[9]Wei W,Wei X,Yang X W.Two new phthalide dimers from the rhizomes of Ligusticum chuanxiong[J].J Asian Nat Prod Res,2017,19(7):1-8.
[10]Chang X L,Jiang Z Y,Ma Y B,et al.Two new compounds from the roots of Ligusticum chuanxiong[J].J Asian Nat Prod Res,2009,11(9):805-810.
[11]陈士林,刘安,李琦,等.中药饮片标准汤剂研究策略[J].中国中药杂志,2016,41(8):1367-1375.
[12]陈素娟,聂静,张旗,等.熟地黄饮片标准汤剂的质量标准研究[J].现代药物与临床,2018,33(9):2173-2177.
[13]张慧,沈潇薇,姜慧洁,等.燀苦杏仁标准汤剂质量与其饮片指标成分苦杏仁苷的相关性探讨[J].中草药,2018,49(9):2063-2069.
[14]李睿,翟华强,田伟兰,等.中药煮散的历史源流及其与现代配方颗粒的对比性分析[J].中国中药杂志,2016,41(5):965-969.
[15]周蔚昕,刘涛,张佳,等.川芎饮片标准汤剂指纹图谱研究[J].中草药,2018,49(10):2401-2409.
[16]崔文金,焦梦姣,邓哲,等.黄连饮片标准汤剂的制备及质量标准分析[J].中国实验方剂学杂志,2017,23(9):40-45.
[17]刘冲,刘荫贞,乐智勇,等.桂枝饮片标准汤剂质量标准研究[J].中草药,2017,48(8):1577-1583.
[18]崔向龙,徐冰,张毅,等.质量源于设计在银杏叶片制粒工艺中的应用(I):颗粒粉体学性质综合评价[J].中国中药杂志,2017,42(6):1037-1042.
[19]李鹏程,刘涛,张文文,等.基于Qb D理念的黄槐片制备工艺及物理指纹图谱研究[J].中草药,2018,49(7):1576-1582.
[20]European Pharmacopeia.Dosage forms monographs[S].2013.
[21]中国药典[S].四部.2015.
[22]张毅,徐冰,孙飞,等.中药提取物粉末物理指纹谱研究及应用[J].中国中药杂志,2016,41(12):2221-2227.
[23]李远辉,伍振峰,李延年,等.基于粉体学性质分析浸膏干燥工艺与中药配方颗粒制粒质量的相关性[J].中草药,2017,48(10):1930-1935.
[24]徐玉玲,谢敏,梁悦,等.基于Qb D理念优选川明参口含片的制备工艺[J].中国实验方剂学杂志,2018,24(17):1-6.
[25]仝家羽,赵嵘,代云桃,等.当归标准汤剂质量评价体系的建立[J].中国实验方剂学杂志,2017,23(7):18-23.
[26]方雯雯,成守玲,陈培胜,等.白芷药材-饮片-提取物及配方颗粒的HPLC特征图谱相关性研究[J].中草药,2016,47(18):3211-3214.
[27]杨胤,冯怡,徐德生,等.干燥工艺与中药提取物物理性质的相关性研究[J].中国药学杂志,2008,43(17):1295-1299.
[28]辜勇军,王广为,王莉,等.不同干燥方法对五龙颗粒浸膏品质的影响[J].中国新药杂志,2015,24(16):1911-1915.