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目的:采用高效液相法同时测定哈蟆油中4-胆甾烯-3-酮和胆固醇。方法:使用Agilent TC-C18柱(4.6 mm×250 mm,5μm),流动相甲醇-水(91.5∶8.5),柱温35℃,体积流速1.0 mL·min-1,检测波长215 nm,进样量10μL。结果:哈蟆油中4-胆甾烯-3-酮进样量在0.011 65~0.116 5μg呈良好的线性关系,平均回收率为100.0%,RSD 1.83%(n=6),且稳定性、精密度及重复性均良好;胆固醇进样量在2.282~22.82μg成良好的线性关系,平均回收率为99.3%,RSD 1.19%(n=6),且稳定性、精密度及重复性均良好。结论:该方法能够同时、准确、稳定、快速的测定哈蟆油中4-胆甾烯-3-酮和胆固醇的含量。
Objective: Simultaneous determination of 4-cholesten-3-one and cholesterol in Rana oil by HPLC. METHODS: The mobile phase was methanol-water (91.5: 8.5), the temperature was 35 ℃ and the flow rate was 1.0 mL · min-1 on an Agilent TC-C18 column (4.6 mm × 250 mm, 5 μm) Amount of 10 μL. Results: The volume of 4-cholesten-3-one in Rana oil was linear with the mass fraction of 0.011 65 ~ 0.116 5μg with the average recovery of 100.0% and RSD 1.83% (n = 6). The stability, The precision and reproducibility were good. The linearity of cholesterol injection was 2.282 ~ 22.82μg, the average recovery was 99.3%, RSD 1.19% (n = 6), and the stability, precision and reproducibility were good . Conclusion: This method can simultaneously, accurately, stably and rapidly determine the content of 4-cholesten-3-one and cholesterol in Rana oil.