HPLC-MS法同时测定酸枣仁中9种成分.PDFVIP

中草药 Chinese Traditional and Herbal Drugs 第 46 卷 第 1 期 2015 年 1 月 • 123 • HPLC-MS 法同时测定酸枣仁中 9 种成分 张巧月，杨浩天，史 贺，张智勇，张兰桐* 河北医科大学药学院 药物分析教研室，河北 石家庄 050017 摘 要：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。 关键词：酸枣仁；HPLC-MS；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 中图分类号：R286.6 文献标志码：A 文章编号：0253 - 2670(2015)01 - 0123 - 05 DOI: 10.7501/j.issn.0253-2670.2015.01.024 Simultaneous quantification of nine constituents in Ziziphi Spinosae Semen by HPLC-MS ZHANG Qiao-yue, YANG Hao-tian, SHI He, ZHANG Zhi-yong, ZHANG Lan-tong Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang 050017, China Abstract: 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 C column 18 (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 ℃ .