HPLC法测定3个产地酸枣仁中斯皮诺素和酸枣仁皂苷A、B的含量

目的:建立HPLC法测定吉林省常用的3个不同产地酸枣仁中斯皮诺素和酸枣仁皂苷A、B的含量,比较其含量差异,为对酸枣仁药材的选择提供依据。方法:采用Eclipse XDB-C₁₈色谱柱(250 mm×4.6 mm,5 μm),柱温30 ℃。以乙腈-水为流动相梯度洗脱,检测波长为335 nm,检测斯皮诺素;以乙腈-水(34:66)为流动相,检测波长为203 nm,同时检测酸枣仁皂苷A和B的含量。结果:斯皮诺素进样量在0.40~4.00 μg(R²=0.999 6)范围内呈良好的线性关系,精密度、稳定性、重现性好,平均加样回收率为98.35%(RSD=1.52%);酸枣仁皂苷A和酸枣仁皂苷B进样量分别在0.48~4.80 μg(R²=0.999 3)和0.24~2.40 μg(R²=0.999 9)范围内呈现良好的线性关系,平均加样回收率分别为98.99%(RSD=0.53%)和98.89%(RSD=0.69%)。3种酸枣仁中进口酸枣仁斯皮诺素含量最高,2种国产酸枣仁样品相差不大;然而,河北省产的酸枣仁皂苷A和B含量最高,其次是山西省,进口酸枣仁含量最低。结论:本文结果表明首次建立的梯度洗脱检测斯皮诺素含量方法准确、可靠,重复性好,可用于评价酸枣仁中斯皮诺素的含量。综合考虑,河北省产的酸枣仁可作为患者的首选药材。

Objective:To establish an HPLC method for content determination of spinosin,jujubosides A and B in Ziziphi Spinosae Semen from three different origins that were mainly sold in each big pharmacy of Jilin province,and to provide scientific evidence for selection of Ziziphi Spinosae Semen.Methods:The assay of spinosin was performed on an Eclipse XDB-C₁₈ column(250 mm×4.6 mm,5 μm)by a new gradient elution program with acetonitrile-water.The column temperature was 30 ℃ and the detection wavelength of UV was 335 nm.Meanwhile,the HPLC-UV method was also used to detect contents of jujubosides A and B with mobile phase of acetonitrile-water(34:66)and detection wavelength of 203 nm.Results:For spinosin,there was a good linear relationship in the range of 0.40-4.00 μg(R²=0.999 6),and the average recovery was 98.35%,with RSD 1.52%.In addition,its precision,stability and reproducibility were also good.The linear ranges of jujubosides A and B were 0.48-4.80 μg(R²=0.999 3)and 0.24-2.40μg(R²=0.999 9)respectively,and the average recovery was 98.99% and 98.89%,with RSD of 0.53% and 0.69%.The highest content of spinosin was the Ziziphi Spinosae Semen in Burma,followed by Shanxi province and Hebei province,which were similar.The highest content of jujubosides A and B was the Semen in Hebei province,followed by Shanxi province,while the lowest was the Semen in Burma.Conclusion:The established method was accurate,reliable,and with good repeatability for detecting spinosin.Simultaneously considering the three typical components,Ziziphi Spinosae Semen in Hebei province could be the best choice for patients.