目的 建立HPLC-MS/MS法同时测定酸枣仁中酸枣仁皂苷A、酸枣仁皂苷B、斯皮诺素、白桦脂酸、白桦脂醇、芦丁、芹菜素、橙皮苷、柚皮苷的量.方法 采用Sapphire C₁₈柱(150 mm×4.6 mm,5 μm),以水(1 mmol/L乙酸铵-0.1%的甲酸)-乙腈溶液为流动相进行梯度洗脱,体积流量1 mL/min,进样量10 μL,柱温30 ℃;采用电喷雾离子源进行负离子模式监测,多反应监测模式(MRM)用于定量分析,源喷射电压为-4 500 V,离子源温度为650 ℃.结果 9种成分的峰面积和质量浓度在测定质量浓度范围内均具有良好的线性关系,加样回收率为98.04%～101.5%,精密度RSD值为0.03%～0.74%.结论 本法简便、快速、灵敏度高、专属性好,可用于酸枣仁中9种化学成分的测定.

Objective To develop an HPLC-MS/MS method for the determination of jujuboside A, jujuboside B, spinosin, betulinic acid, betulin, rutin, apigenin, hesperidin, and naringin in Ziziphi Spinosae Semen. Methods Analysis was performed on a Sapphire C₁₈ column (150 mm × 4.6 mm, 5 μm) eluted with acetonitrile and 0.1% methanoic acid solution containing 1 mmol/L ammonium acetate in a gradient program. The flow rate was 1 mL/min, the injection volume was 10 μL, and the column temperature was 30 ℃. The multiple-reaction monitoring scanning (MRM) was employed for the quantification with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at -4 500 V and the turbo spray temperature was maintained at 650 ℃. Results The regression equations showing linear relationships between peak areas and contents of each compound were obtained. The average recoveries of the compounds ranged from 98.04% to 101.5% and the precision in terms of RSD was in the range of 0.03%—0.74%. Conclusion The method is simple, rapid, and sensitive. It could be used as a quantitative determination method for the nine components in Ziziphi Spinosae Semen.

河北省自然基金-石药集团医药联合研究基金(H2012206079)