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.
作者
唐德智
TANG De-zhi(Guangxi Nanning Institute for Food and Drug Control, Nanning 530001, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2016年第10期1870-1874,共5页
Chinese Journal of Pharmaceutical Analysis
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
Fufang Huangqin tablets
Scutellariae Radix
Polygoni Cuspidati Rhizoma et Radix
Andrographis Herba
polydatin
baicalin
wogonoside
baicalein
andrographolide
dehydroandrographolide
multicomponent assay of traditional Chinese patent medicines
methods validation
wavelength switching method
HPLC
