甲肿消制剂及其含药血清中哈巴俄苷的含量测定

目的 建立甲肿消制剂及灌胃给予甲肿消后大鼠血清中的哈巴俄苷含量测定方法.方法 采用RP-HPLC法测定哈巴俄苷的含量,色谱柱:Kromasil C_(18)色谱柱(250 mm×4.6 mm,5 μm)和Easyguard保护柱,以乙腈和1%醋酸溶液为流动相,采用梯度洗脱;流速:1 ml· min~(-1);检测波长为278 nm;进样量:5 μl.结果 哈巴俄苷在1.46～146 μg·ml~(-1)的浓度范围内线性良好;低、中、高浓度哈巴俄苷的精密度(RSD)(n=5)分别为1.05%,0.59%,0.80%;日间差(RSD)(n=5)为1.00%;制剂和大鼠血清中哈巴俄苷的加样回收率(n=5)分别为(98.02±1.01)%和(101.03±1.64)%;测定其重现性(RSD)(n=6)分别为0.73%和0.96%;每克制剂中含哈巴俄苷的量为230.5 μg,每毫升含药血清中哈巴俄苷的量为1.88 μg.结论 该方法简便、快速、准确、重现性良好,可用于制剂和血清中哈巴俄苷的含量测定.

Determination of Harpagoside in Jia Zhong Xiao Preparation and Rat Serum

Objective To develop a determination method of Harpagoside in Jia Zhong Xiao preparation and blood serum of rat. Methods The RP-HPLC method was applied as with: Kromasil C_(18) column(250 mm×4.6 mm,5 μm) and Easyguard column.The mobile phase was acetonitrile and 1% acetic acid with linearity gradient elution,the flow rate at 1 ml·min~(-1), and detection wavelength was 278nm. Results An excellent linearity was obtained over the range of 1.46～146 μg·ml~(-1). The RSDs of accuracy for 7.3, 29.2, 146μg·ml~(-1) were 1.05%,0.59%,0.80%, respectively (n=5). The RSDs of intra-day validation were 1.00%. The mean recovery rates of Harpagoside in preparation and serum were (98.02±1.01)%, (101.03±1.64)%,respectively. The RSDs of the determination method for preparation and serum repeatability were 0.73% and 0.96%, respectively. The content of Harpagoside in preparation and serum was 230.5μg·g~(-1) and 1.88μg·ml~(-1), respectively.Conclusion The method is simple, rapid, reliable and repeatable. It's quite suitable for the analysis of Harpagoside in Jia Zhong Xiao preparation and of rat serum.