生/醋延胡索饮片及配方颗粒的指纹图谱研究及5种生物碱的含量测定
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篇名: 生/醋延胡索饮片及配方颗粒的指纹图谱研究及5种生物碱的含量测定
TITLE: Study on the Fingerprint of Crude/vinegar-processed Corydalis yanhusuo Decoction Pieces and Their Dispen- sing Granules and Content Determination of Five Alkaloids
摘要: 目的:建立生/醋延胡索饮片及配方颗粒的指纹图谱,并测定其中5种生物碱成分(原阿片碱、延胡索乙素、延胡索甲素、盐酸小檗碱、盐酸巴马汀)的含量。方法:采用高效液相色谱法。色谱柱为AgilentTC-C18,流动相为0.1%磷酸水溶液-甲醇(梯度洗脱),流速为1.0mL/min,检测波长为280nm,柱温为30℃,进样量为10μL。以盐酸巴马汀为参照,利用《中药色谱指纹图谱相似度评价系统(2012版)》建立11批生延胡索饮片、7批生延胡索配方颗粒、12批醋延胡索饮片、11批醋延胡索配方颗粒的指纹图谱并进行相似度评价;采用上述HPLC法测定41批生/醋延胡索饮片及配方颗粒中原阿片碱、延胡索乙素、延胡索甲素、盐酸小檗碱、盐酸巴马汀的含量。结果:生延胡索饮片及其配方颗粒分别确定共有峰12、20个,醋延胡索饮片及其配方颗粒分别确定共有峰14、16个;各批次同类样品的相似度分别为0.529~0.981、0.342~0.985、0.711~0.999、0.437~0.998。原阿片碱、延胡索乙素、延胡索甲素、盐酸小檗碱、盐酸巴马汀检测质量浓度的线性范围分别为1.9~38.0、2.0~40.0、2.2~44.0、2.6~52.0、2.3~46.0μg/mL(R2均大于0.9990),加样回收率为100.12%~100.98%(RSD=1.05%~1.90%,n=9),精密度、重复性、稳定性(24h)、耐用性试验的RSD均小于2.0%。不同批次的生/醋延胡索饮片及配方颗粒中上述5种生物碱成分的平均含量分别为0.24~0.46、0.37~0.82、0.24~0.58、0.07~0.75、0.24~0.76mg/g,RSD为12.27%~147.48%。结论:成功建立生/醋延胡索饮片及配方颗粒的指纹图谱;醋制前后延胡索饮片及配方颗粒指纹图谱相似度不一,且其中上述5种生物碱含量差异较大。
ABSTRACT: OBJECTIVE:To establish the fingerprint of crude/vinegar-processed Corydalis yanhusuo decoction pieces and their dispensing granules,and to determine the contents of five alkaloids (protopine,tetrahydropalmatine,corydaline,berberine hydrochloride,palmatine hydrochloride ). METHODS :HPLC method was adopted. The determination was performed on Agilent TC-C18 column with mobile phase consisted of 0.1% phosphoric acid solution-methanol (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelength was set at 280 nm,and the column temperature was 30 ℃. The sample size was 10 μL. Using palmatine hydrochloride as reference , Similarity Evaluation System of TCM Chromatographic Fingerprint (2012 edition) was used to establish the fingerprint of 11 059) batches of C. yanhusuo decoction pieces ,7 batches of crude . yanhusuo dispensing granules , 12 batches of vinegar- processed C. yanhusuo decoction pieces and 11 batches of vinegar-processed C. yanhusuo dispensing granules. The same HPLC method was adopted to determine the contents of protopine, tetrahydropalmatine, corydaline, berberine hydrochloride and palmatine hydrochloride in 41 batches of crude/ vinegar-processed C. yanhusuo decoction pieces and their dispensing granules. RESULTS :There were 12 and 20 common peaks for crude C. yanhusuo decoction pieces and its dispensing granules ,and 14 and 16 common peaks for vinegar-processed C. yanhusuo decoction pieces and its dispensing granules. The similarity of each batch of same type were 0.529-0.981,0.342-0.985, 0.711-0.999,0.437-0.998,respectively. The linear range of protopine ,tetrahydropalmatine,corydaline,berberine hydrochloride and palmatine hydrochloride were 1.9-38.0,2.0-40.0,2.2-44.0,2.6-52.0,2.3-46.0 μg/mL(R2>0.999 0). The recoveries were 100.12%-100.98%(RSD=1.05%-1.90%,n=9). RSDs of precision ,reproducibility,stability(24 h)and durability tests were all lower than 2.0%. The average contents of five alkaloids in different batches of crude/vinegar-processed C. yanhusuo decoction pieces and its dispensing granules were 0.24-0.46,0.37-0.82,0.24-0.58,0.07-0.75,0.24-0.76 mg/g. RSDs were 12.27%-147.48%. CONCLUSIONS:The fingerprint of crude/vinegar-processed C. yanhusuo decoction pieces and its dispensing granules is established successfully. The similarities of fingerprint are different before and after processing with vinegar ,and the contents of five alkaloids in C. yanhusuo decoction pieces and its dispensing granules are greatly different.
期刊: 2020年第31卷第20期
作者: 孙萍萍,郭正红,杨武德,羊波,沈成俊,沈祥春,陶玲,肖婷
AUTHORS: SUN Pingping, GUO Zhenghong,YANG Wude,YANG Bo,SHEN Chengjun,SHEN Xiangchun,TAO Ling,XIAO Ting
关键字: 延胡索;醋制;高效液相色谱法;生物碱;指纹图谱;含量测定
KEYWORDS: Corydalis yanhusuo ;Vinegar-procession;HPLC;Alkaloids;Fingerprint;Content determination
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