[关键词]
[摘要]
目的 建立UPLC-MS/MS法同时测定香砂平胃颗粒中苍术素、厚朴酚、和厚朴酚、橙皮苷、芸香柚皮苷和甘草苷。方法 色谱条件采用Waters HSS T3 C18色谱柱(100 mm×2.1 mm,1.7 μm),流动相为乙腈-0.1%甲酸水,梯度洗脱,体积流量0.3 mL/min,柱温40 ℃,进样量5 μL。质谱条件选择离子源:电喷雾离子源(ESI),采集模式:多反应检测(MRM),正负离子同时扫描,离子源温度150 ℃,毛细管电压:正离子3.0 kV,负离子2.5 kV,去溶剂气流量800 L/h,去溶剂气温度400 ℃,氩气为高纯氩气。结果 甘草苷、芸香柚皮苷、橙皮苷、和厚朴酚、厚朴酚、苍术素线性范围在0.29~14.75、0.38~18.58、1.85~92.63、1.62~81.11、1.37~68.5、0.49~24.41 ng,平均回收率分别为100.48%、97.79%、98.67%、93.52%、101.72%、100.30%,RSD值分别为4.31%、3.40%、1.45%、2.78%、2.59%、4.06%。结论 本法分析速度快、灵敏度高、专属性强,可以为香砂平胃颗粒的质量标准改进提供依据。
[Key word]
[Abstract]
Objective To develop an UPLC-MS/MS method for the simultaneous determination of atractylodin, honokiol, magnolol, hesperidin, naringin, and liquiritin in Xiangsha Pingwei Granules. Methods The chromatographic condition was Waters HSS T3 C18 column (100 mm × 2.1 mm, 1.7 μm), mobile phase acetonitrile -0.1% formic acid solution with gradient elution, column temperature set at 40 ℃, and injection volume of 5 μL with flow rate of 0.3 mL/min. The mass spectrum condition with ESI ions source, acquisition mode: MRM, simultaneous scanning of positive and negative ions, ion source temperature 150 ℃, capillary voltage: positive ions 3.0 kV, negative ions 2.5 kV, desolvent gas flow 800 L/h, desolvent gas temperature 400 ℃, and argon as high-purity argon. Results Liquiritin, naringin, hesperidin, magnolol, honokiol, and atractylodin showed good linear relationships in the concentration range of 0.29-14.75, 0.38-18.58, 1.85-92.63, 1.62-81.11, 1.37-68.5, and 0.49-24.41 ng. The average recoveries were 100.48%, 97.79%, 98.67%, 93.52%, 101.72%, and 100.30% with RSD values of 4.31%, 3.40%, 1.45%, 2.78%, 2.59%, and 4.06%, respectively. Conclusion The method is fast, sensitive, and specific, and can provide a basis for improving the quality standard of Xiangsha Pingwei Granules.
[中图分类号]
R286.02
[基金项目]