通络止痛胶囊中4种成分测定及HPLC指纹图谱建立

目的测定通络止痛胶囊(虎杖、当归、独活等)中4种成分的含有量,并建立HPLC指纹图谱。方法该药物甲醇提取液的分析采用Waters XSelect C₁₈色谱柱(4.6 mm×250 mm,5μm);流动相甲醇-0.5%磷酸,梯度洗脱;体积流量1.0 mL/min;柱温25℃;检测波长330 nm。以虎杖苷为内标,计算其他3种成分的相对校正因子,一测多评法测定含有量。结果虎杖苷、阿魏酸、蛇床子素、二氢欧山芹醇当归酸酯分别在16.61～332.16、1.07～21.42、15.66～313.15、24.91～498.21μg/mL范围内线性关系良好(r>0.999 0),平均加样回收率分别为100.01%、99.47%、99.63%、99.06%,RSD分别为0.42%、1.85%、0.54%、0.87%。一测多评法所得结果与外标法接近。10批样品指纹图谱中有21个共有峰,相似度大于0.950。结论该方法简便高效,重复性好,可用于通络止痛胶囊的质量控制。

Determination of four constituents in Tongluo Zhitong Capsules and establishment of HPLC fingerprints

AIM To determine the contents of four constituents in Tongluo Zhitong Capsules(Polygoni cuspidati Rhizoma et Radix,Angelicae sinensis Radix,Angelicae pubescentis Radix,etc.)and to establish the HPLC fingerprints.METHODS The analysis of methanol extract of this drug was performed on a 25℃thermostatic Waters XSelect C18 column(4.6 mm×250 mm,5μm),with the mobile phase comprising of methanol-0.5%phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 330 nm.Polydatin was used as an internal standard to calculate the relative correction factors of the other three constituents,after which the content determination was made by quantitative analysis of multi-components by single-marker(QAMS).RESULTS Polydatin,ferulic acid,osthole,columbianadin showed good linear relationships within the ranges of 16.61-332.16,1.07-21.42,15.66-313.15,24.91-498.21μg/mL(r>0.9990),whose average recoveries were 100.01%,99.47%,99.63%,99.06%with the RSDs of 0.42%,1.85%,0.54%,0.87%,respectively.The results obtained by QAMS approximated those obtained by external standard method.There were twenty-one common peaks in the fingerprints of ten batches of samples with the similarities of more than 0.950.CONCLUSION This simple,efficient and reproducible method can be used for the quality control of Tongluo Zhitong Capsules.