摘要
目的建立同时测定桂芍镇痫片中8种成分氧化芍药苷、芍药内酯苷、芍药苷、苯甲酰芍药苷、肉桂酸、桂皮醛、柴胡皂苷a和柴胡皂苷d的一测多评方法。方法采用HPLC法,Thermo ODS C18(250 mm×4.6 mm,5μm)色谱柱,乙腈-0.1%磷酸溶液为流动相,梯度洗脱,体积流量1.1 m L/min,柱温25℃。建立氧化芍药苷、芍药内酯苷、苯甲酰芍药苷、肉桂酸、桂皮醛、柴胡皂苷a和柴胡皂苷d与内标芍药苷的相对校正因子,通过相对校正因子计算桂芍镇痫片中8种成分的含量,与外标法测定的结果进行对比分析,以验证一测多评法的合理性、可行性和重复性。结果氧化芍药苷、芍药内酯苷、芍药苷、苯甲酰芍药苷、肉桂酸、桂皮醛、柴胡皂苷a和柴胡皂苷d的线性范围分别为2.63~65.75μg/m L(r=0.999 7)、9.67~241.75μg/m L(r=0.999 8)、13.59~339.75μg/m L(r=0.999 5)、1.79~44.75μg/m L(r=0.999 4)、2.45~61.25μg/m L(r=0.999 1)、7.98~199.50μg/m L(r=0.999 7)、2.79~69.75μg/m L(r=0.999 3)、2.51~62.75μg/m L(r=0.999 5);平均加样回收率分别为98.64%、99.33%、100.02%、97.42%、96.95%、98.75%、98.21%、97.81%,RSD分别为0.89%、1.19%、1.00%、1.33%、1.51%、0.99%、1.43%、0.80%;氧化芍药苷、芍药内酯苷、苯甲酰芍药苷、肉桂酸、桂皮醛、柴胡皂苷a和柴胡皂苷d与内标物芍药苷的相对校正因子分别为0.520 9、1.086 9、0.476 8、0.626 1、0.802 1、0.713 8、0.367 0;一测多评法的计算结果与外标法的实测值无显著性差异。结论建立的一测多评法可作为一种简便准确的质量评价模式用于桂芍镇痫片中氧化芍药苷、芍药内酯苷、芍药苷、苯甲酰芍药苷、肉桂酸、桂皮醛、柴胡皂苷a和柴胡皂苷d的质量控制。
Objective To establish a quantitative analysis of multi-components with a single-marker（QAMS） method for the simultaneous determination of oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin, cinnamic acid, cinnamaldehyde, saikosaponin a, and saikosaponin d in Guishao Zhenxian Tablets（GZT）. Methods The separation was performed on a Thermo ODS C18 column（250 mm × 4.6 mm, 5 μm）, with the mobile phase consisting of acetonitrile-0.1% phosphate acid solution for gradient elution. The column temperature was 25 ℃, and flow rate was 1.1 m L/min. Using paeoniflorin as internal reference substance, the relative correlation factors of oxypaeoniflorin, albiflorin, benzoylpaeoniflorin, cinnamic acid, cinnamaldehyde, saikosaponin a, and saikosaponin d were calculated and established by HPLC. The results were compared with those obtained by the external standard method to verify the rationality, feasibility, and repeatability of QAMS method. Results Oxypaeoniflorin, albiflorin, paeoniflorin, benzoylpaeoniflorin, cinnamic acid, cinnamaldehyde, saikosaponin a, and saikosaponin d had good relations within the ranges of 2.63—65.75 μg/m L（r = 0.999 7）, 9.67—241.75 μg/m L（r = 0.999 8）, 13.59—339.75 μg/m L（r = 0.999 5）, 1.79—44.75 μg/m L（r = 0.999 4）, 2.45—61.25 μg/m L（r = 0.999 1）, 7.98—199.50 μg/m L（r = 0.999 7）, 2.79—69.75 μg/m L（r = 0.999 3）, and 2.51—62.75 μg/m L（r= 0.999 5）, respectively. The recovery rates were 98.64%, 99.33%, 100.02%, 97.42%, 96.95%, 98.75%, 98.21%, and 97.81%, RSDs were 0.89%, 1.19%, 1.00%, 1.33%, 1.51%, 0.99%, 1.43%, and 0.80%, respectively. The relative correlation factors values of oxypaeoniflorin, albiflorin, benzoylpaeoniflorin, cinnamic acid, cinnamaldehyde, saikosaponin a, and saikosaponin d to paeoniflorin were 0.520 9, 1.086 9, 0.476 8, 0.626 1, 0.802 1, 0.713 8, and 0.367 0, respectively. There were no significant difference in assay results between QAMS and the external standard method. Conclusion The QAMS method is
作者
高森
白雪
文柳静
李正翔
房志仲
GAO Sen;BAI Xue;WEN Liu-jing;LI Zheng-xiang;FANG Zhi-zhong(Department of Pharmacy, General Hospital, Tianjin Medical University, Tianjin 300052, China;State Key Laboratory of Chinese medicine key technology innovation, Traditional Chinese Medicine Development Center, Tasly Holding Group Academy, Tianjin 300402, China;Tianjin Key Lab of Cancer Prevention and Treatment, State Cancer Clinical Medical Research Center, Tianjin Medical University Cancer Hospital, Tianjin 300060, China;Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics, School of Pharmacy, Tianjin Medical University, Tianjin 300070, China)
出处
《中草药》
CAS
CSCD
北大核心
2018年第12期2883-2889,共7页
Chinese Traditional and Herbal Drugs
关键词
一测多评法
相对校正因子
桂芍镇痫片
质量控制
氧化芍药苷
芍药内酯苷
芍药苷
苯甲酰芍药苷
肉桂酸
桂皮醛
柴胡皂苷A
柴胡皂苷D
quantitative analysis of multi-components with a single-marker
relative correlation factors
Guishao Zhenxian Tablets
quality control
oxypaeoniflorin
albiflorin
paeoniflorin
benzoylpaeoniflorin
cinnamic acid
cinnamaldehyde
saikosaponin a
saikosaponin d
