HPLC法测定复方黄芩片中6个成分的含量  

Simultaneous determination of six components in Fufang Huangqin tablets by HPLC

作　　者：唐德智 TANG De-zhi(Guangxi Nanning Institute for Food and Drug Control, Nanning 530001, China)

机构地区：[1]广西南宁食品药品检验所,南宁530021

出　　处：《药物分析杂志》2016年第10期1870-1874,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC波长切换法测定复方黄芩片中虎杖苷、黄芩苷、汉黄芩苷、黄芩素、穿心莲内酯、脱水穿心莲内酯的含量。方法:采用Agilent SB-C_(18)(4.6 mm×150 mm,5μm)色谱柱,流动相为乙腈(A)-0.1磷酸水溶液(B)系统,梯度洗脱,流速为1.0 m L·min^(-1),柱温:30℃,波长切换时间序列采样(0~10 min,306 nm,检测虎杖苷;10~23 min,280 nm,检测黄芩苷;23~25min,225 nm,检测穿心莲内酯;25~33 min,280 nm,检测汉黄芩苷、黄芩素;33~50 min,254 nm,检测脱水穿心莲内酯)。结果:虎杖苷进样量在0.046~0.823μg范围内线性关系良好(r=0.999 9,n=6),平均回收率为99.30%,RSD为1.5%(n=6);黄芩苷进样量在0.468~8.428μg范围内线性关系良好(r=0.999 7,n=6),平均回收率为99.76%,RSD为1.3%(n=6);汉黄芩苷进样量在0.116~2.084μg范围内线性关系良好(r=0.999 9,n=6),平均回收率为100.3%,RSD为1.8%(n=6);黄芩素进样量在0.117~2.110μg范围内线性关系良好(r=0.999 8,n=6),平均回收率为99.25%,RSD为1.3%(n=6);穿心莲内酯进样量在0.029~0.524μg范围内线性关系良好(r=0.999 8,n=6),平均回收率为99.91%,RSD为1.6%(n=6);脱水穿心莲内酯进样量在0.033~0.592μg范围内线性关系良好(r=0.999 7,n=6),平均回收率为99.94%,RSD为1.6%(n=6)。5批样品中虎杖苷、黄芩苷、汉黄芩苷、黄芩素、穿心莲内酯和脱水穿心莲内酯含量范围分别为2.09~2.25、22.74~25.91、5.69~6.08、5.74~6.11、1.27~1.41、1.49~1.69 mg·g^(-1)。结论:该方法经方法学验证,可用于复方黄芩片的质量控制。Objective：To establish an HPLC method for simultaneous determination of polydatin,baicalin,wogonoside,baicalein,andrographolide,and dehydroandrographolide in Fufang Huangqin tablets.Methods：Theseparation was performed on an Agilent SB-C18 column（ 4.6 mm×150 mm,5 μm） with gradient elution at a temperature of 30 ℃.The acetonitrile and 0.1%（v/v） phosphoric acid were used as the mobile phase with a flow rate of 1.0 mL ·min-1.The detection wavelength was 306 nm（0-10 min） for polydatin,280 nm（10-23 min） for baicalin,225 nm（23-25 min） for andrographolide,280 nm（25-33 min） for wogonoside and baicalein,and 254 nm（33-50 min） for dehydroandrographolide.Results：Polydatin had a good linearity in the range of 0.046-0.823 μg,the average recovery was 99.30% with RSD of 1.5%（n=6）;baicalin had a good linearity in the range of 0.468-8.428 μg,the average recovery was 99.76% with RSD of 1.3%（n=6）;wogonoside had a good linearity in the range of 0.116-2.084 μg,the average recovery was 100.3% with RSD of 1.8%（n=6）;baicalein had a good linearity in the range of 0.117-2.110 μg,the average recovery was 99.25% with RSD of 1.3%（ n=6）;andrographolide had a good linearity in the range of 0.029-0.524 μg,the average recovery was 99.91% with RSD of 1.6%（n=6）;dehydroandrographolide had a good linearity in the range of 0.033-0.592 μg,the average recovery was 99.94% with RSD of 1.6%（n= 6）.The contents of polydatin,baicalin,wogonoside,baicalein,andrographolide and dehydroandrographolide in 5 samples were 2.09-2.25,22.74-25.91,5.69-6.08,5.74-6.11,1.27-1.41 and 1.49-1.69 mg·g-1,respectively.Conclusion：The established method is validated by methodology that it is suitable for the quality control of Fufang Huangqin tablets.

关 键 词：复方黄芩片 黄芩 虎杖 穿心莲 虎杖苷 黄芩苷 汉黄芩苷 黄芩素 穿心莲内酯 脱水穿心莲内酯 中成药多成分测定 方法学验证 波长切换法 HPLC 

分 类 号：R917[医药卫生—药物分析学]