机构地区:[1]首都医科大学中医药学院,北京100069 [2]中国中医科学院中药研究所,北京100700 [3]中药质量控制技术国家工程实验室,北京100700
出 处:《中国中药杂志》2015年第10期1865-1871,共7页China Journal of Chinese Materia Medica
基 金:国家"重大新药创制"科技重大专项(2012ZX09304005002);国家药典委员会标准提高暨2015年版<中国药典>科研任务
摘 要:建立大血藤药材中总酚、总皂苷和指标成分红景天苷、绿原酸、3,4-二羟基苯乙醇葡萄糖苷的含量测定方法,为2015版《中国药典》大血藤药材和饮片质量标准修订提供参考。以没食子酸为指标,采用分光光度法测定总酚的含量;以特征性成分3-O-[β-D-木糖基-(1-2)-O-β-D-葡萄糖醛酸基]-28-O-[β-D-葡萄糖基]积雪草酸为指标,采用分光光度法测定总皂苷含量;采用高效液相色谱法测定红景天苷、绿原酸、3,4-二羟基苯乙醇葡萄糖苷的含量。总酚在1.01~7.04 mg·L-1线性关系良好,平均加样回收率为99.12%;总皂苷在37.7~201μg线性关系良好,平均加样回收率为99.11%;红景天苷、绿原酸、3,4-二羟基苯乙醇葡萄糖苷分别在0.025 8~1.55,0.076 2~5.44,0.0649~3.47μg线性关系良好,平均加样回收率分别为105.5%,99.08%,101.6%;大血藤中总酚和总皂苷的质量分数分别为3.04%~11.9%和0.87%~3.63%,红景天苷、绿原酸、3,4-二羟基苯乙醇葡萄糖苷的质量分数分别为0.018%~0.572%,0.041%~1.75%,0.035~1.32%。建立的各指标定量分析方法重复性好,适合用于大血藤药材的质量评价。建议2015年版《中国药典》大血藤药材标准项下增加总酚、红景天苷和绿原酸的含量测定方法,以干燥品计,含总酚以没食子酸(C7H8O6)计不得少于6.8%;含红景天苷(C14H20O7)不得少于0.040%,含绿原酸(C16H18O9)不得少于0.21%。The methods to determine the total phenols, total saponins, and marker constituents salidroside, chlorogenic acid and 3, 4-dihydroxy-phenylethy158-D-glucopyranoside in the samples of Sargentodoxae Caulis were established to provide the evidence for the improvement and revision of the quality standard of the crude material recorded in the Chinese Pharmacopoeia(2015 Edition). The content of total phenols was determined by ultraviolet spectrophotometry, using gallic acid as a reference substance. The content of total saponins was determined by ultraviolet spectrophotometry, using 3-O- β-D-xylopyranosyl- (1-2) -O-β-D-glucuronopyranosyl ] -28-O- β- D- glueopyranosyl ] asiatic acid as a reference substance. The contents of salidroside, chlorogenic acid and 3,4-dihydroxy-phenylethy-β-D-glucopyranoside were detected by HPLC. The linear ranges were 1.01-7.04 mg· L^- 1 for total phenols, 37.7-201 txg for total saponins, 0. 025 8-1.55 βg for salidroside, 0. 076 2-5.44 μg for chlorogenic acid, and 0.064 9-3.47 μg for 3,4-dihydroxy-phenylethyl- β-D-glucopyranoside, respectively. Their average recoveries were 99.12%, 99.11% 105.5%, 99.08%, and 101.6%, respectively. The contents of total phenols and total saponins were 3.04% -11.9% and 0.87%-3.63 %. The contents of salidroside, chlorogenic acid and 3,4-dihydroxy-phenylethyl-β-D-glucopyranoside fluctuated from 0. 018% to 0. 572%, from 0. 041% to 1.75% and from 0. 035% to 1.32%. The established methods were reproducible, and they could be used for the quality control of Sargentodoxae Caulis. The present investigation suggested that total phenols, salidroside, and chlorogenic acid should be recorded in the quality standard of Sargentodoxae Caulis and their contents should not be less than 6. 8% for total phenols, 0. 040% for salidroside, and 0. 21% for chlorogenic acid.
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