摘要
目的:建立赤芍-当归药对中没食子酸、氧化芍药苷、香草酸、芍药内酯苷、芍药苷、阿魏酸、1,2,3,4,6-O-五没食子酰葡萄糖、苯甲酰芍药苷、丹皮酚、藁本内酯10个成分的含量测定方法,考察不同配伍比例及配伍方式对赤芍-当归药对中10个主要活性成分溶出量的影响。方法:采用Wonda Cract ODS-2色谱柱(4.6mm×250 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速1.0 mL·min-1,柱温25℃,变换波长检测赤芍-当归药对中10个成分,检测波长为210、230、260、274、275、325、350 nm。进一步测定赤芍-当归药对的单煎液、单煎合并液(1∶1)以及不同配比的合煎液(1∶1,1∶2,1∶3,2∶1,3∶1)中上述10个主要活性成分的含量。结果:没食子酸、氧化芍药苷、香草酸、芍药内酯苷、芍药苷、阿魏酸、1,2,3,4,6-O-五没食子酰葡萄糖、苯甲酰芍药苷、丹皮酚、藁本内酯质量浓度分别在1.49~74.50μg·m L-1(r=0.996 0)、2.88~144.00μg·m L-1(r=0.996 4)、2.96~147.99μg·m L-1(r=0.997 6)、2.94~147.00μg·m L-1(r=0.997 9)、2.99~149.50μg·m L-1(r=0.998 1)、2.24~111.99μg·m L-1(r=0.997 8)、3.01~150.50μg·m L-1(r=0.997 8)、2.98~148.99μg·m L-1(r=0.998 4)、2.79~139.50(r=0.997 3)、6.00~300.00(r=0.998 2)μg·m L-1范围内与峰面积呈良好的线性关系。精密度良好,RSD小于2.0%;回收率良好,3个加样浓度的平均回收率(n=9)为83.7%~100.4%,RSD为2.5%~7.2%。当赤芍-当归比例为2∶1时,各成分含量明显大于单煎液中含量,且多种成分在该比例中含量最高。当赤芍-当归比例为1∶1时,合煎液中含量较高的5个成分的溶出量明显多于单煎合并液。结论:本研究所建立的测定方法,结果可靠准确,操作简便,可用于赤芍-当归药对中10个成分的含量测定;赤芍-当归(2∶1)的配伍比例以及合煎的配伍方式有利于10个成分在水中的溶出。
Objective:To establish a method for simultaneous determination of ten components(gallic acid,oxypaeoniflorin,vanillic acid,albiflorin,paeoniflorin,ferulic acid,1,2,3,4,6-penta-O-galloy-β-D-glucose,benzoylpaeoniflorin,paeonol,ligustilide)in Paeoniae Radix Rubra and Angelicae Sinensis Radix drug pair,and to study the influence of compatibility proportions on the ten components.Methods:A Wonda Cract ODS-2 column(250 mm×4.6 mm,5μm)was used for the separation,with gradient elution of acetonitrile and 0.1%phosphoric acid as the mobile phase at a flow rate of 1.0 m L·min-1.The detection wavelength was set at 210,230,260,274,275,325 and 350 nm.The column temperature was 25℃.And the ten components were determined in different compatibility proportions,including single decoction,mixed single decoctions(1∶1)and mixed decoction(1∶1,1∶2,1∶3,2∶1 and 3∶1).Results:The linear range was 1.49-74.50μg·m L-1 for gallic acid(r=0.996 0),2.88-144.00μg·m L-1 for oxypaeoniflorin(r=0.996 4),2.96-147.99μg·m L-1 for vanillic acid(r=0.997 6),2.94-147.00μg·m L-1 for albiflorin(r=0.997 9),2.99-149.50μg·m L-1 for peaoniflorin(r=0.998 1),2.24-111.99μg·m L-1 for ferulic acid(r=0.997 8),3.01-150.50μg·m L-1 for 1,2,3,4,6-penta-O-galloy-β-D-glucose(r=0.997 8),2.98-148.99μg·m L-1 for benzoylpaeoniflorin(r=0.998 4),2.79-139.50μg·m L-1 for paeonol(r=0.997 3),and 6.00-300.00μg·m L-1 for ligustilide(r=0.998 2).The results of the precision tests were satisfactory with relative standard deviations(RSDs)all below 2.0%.The average spike recoveries(n=9)at three concentration levels were 83.7%-100.4%,with RSDs within 2.5%-7.2%.Compared with the single decoction,when the proportion of Paeoniae Radix Rubra-Angelicae Sinensis Radix(m/m)was 2∶1,the contents of the ten components increased obviously in mixed decoction.And the contents of most of ten components were the highest in the 2∶1 drug pair.Compared with the mixed single decoctions,the contents of oxypaeoniflorin,vanillic acid,albiflorin,peaoniflorin and paeonol incr
作者
程江雪
唐志书
郭东艳
史亚军
邹俊波
王晶
王鹏
CHENG Jiang-xue;TANG Zhi-shu;GUO Dong-yan;SHI Ya-jun;ZOU Jun-bo;WANG Jing;WANG Peng(College of Pharmacy,Shaanxi University of Chinese Medicine,Xianyang712046,China;Shaanxi Province Key Laboratory of Basic and New Herbal Medicament Research,Xianyang712046,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第9期1597-1604,共8页
Chinese Journal of Pharmaceutical Analysis
基金
陕西省教育厅专项科研计划项目(18JK0231)
陕西中医药大学学科创新团队建设项目(No.2019-YL11)
关键词
赤芍
当归
单煎
合并
合煎
高效液相色谱法
配伍
含量测定
Paeoniae Radix Rubra
Angelicae Sinensis Radix
single decoction
mixed single decoctions
mixed decoction
HPLC
compatibility
content determination
