UPLC-DAD-ELSD切换波长法同时测定复方酸枣仁颗粒中8种成分的含量

目的：建立UPLC-DAD-ELSD切换波长法测定酸枣仁颗粒中芒果苷、阿魏酸、甘草苷、斯皮诺素、知母皂苷B Ⅱ、酸枣仁皂苷A、白桦脂酸、白桦脂醇的含量。方法：采用Agilent Zorbax Eclipse plus C₁₈色谱柱（2.1 mm×50 mm，1.8 μm），流动相为乙腈-0.1%醋酸溶液，梯度洗脱，流速0.4 mL·min^-1，检测波长250 nm（0~5.8 min，芒果苷，阿魏酸）、280 nm（5.8~25 min，甘草苷，斯皮诺素），柱温40℃；蒸发光散射检测器（知母皂苷B Ⅱ、酸枣仁皂苷A、白桦脂酸、白桦脂醇），雾化器温度为40℃，漂移管温度为100℃，气体流速1.60 L·min^-1。结果：各待测组分分离度良好；芒果苷、阿魏酸、甘草苷、斯皮诺素、知母皂苷B Ⅱ、酸枣仁皂苷A、白桦脂酸、白桦脂醇的进样量分别在0.021~0.412 μg（r=0.999 9）、0.004~0.083 μg（r=0.999 0）、0.020~0.402 μg（r=0.999 9）、0.019~0.348 μg（r=0.999 9）、0.094~1.890 μg（r=0.999 0）、0.020~0.410μg（r=0.999 2）、0.051~1.025 μg（r=0.999 1）和0.013~0.270 μg（r=0.999 5）范围内与各自峰面积呈良好线性关系；芒果苷含量为0.534~0.911 mg·g^-1，阿魏酸含量为0.114~0.213 mg·g^-1，甘草苷含量为0.534~0.552 mg·g^-1，斯皮诺素含量为0.641~0.733 mg·g^-1，知母皂苷B Ⅱ含量为1.066~1.208 mg·g^-1，酸枣仁皂苷A含量为0.644~0.845 mg·g^-1，白桦脂酸含量为2.181~2.211 mg·g^-1，白桦脂醇含量为0.307~0.309 mg·g^-1。结论：经方法学验证，本法可用于复方酸枣仁颗粒的质量控制。

Objective: To establish a method for simultaneous determination of mangiferin,ferulic acid,liquiritin, spinosin, timosaponin B Ⅱ, jujuboside A, betulinic acid, betulin in compound Semen Ziziphi Spinoase granules by UPLC-DAD-ELSD wavelength switching. Methods: Agilent Zorbax Eclipse plus chromatographic column(2.1 mm×50 mm, 1.8 μm)was adopted. The mobile phase was acetonitrile -0.1% acetic acid with gradient elution at a flow rate of 0.4 mL·min^-1. The detection wavelength was 250 nm(0-5.8 min, for mangiferin and ferulic acid), 280 nm(5.8-25 min, for liquiritin, spinosin). The column temperature was 40℃. The nebulizer temperature of ELSD for timosaponin B Ⅱ, jujuboside A, betulinic acid and betulin was maintained at 40℃, the drift tube temperature was 100℃ and the gas flow rate was maintained at 1.60 L·min^-1. Results: The complete separation of 8 compounds was obtained. The method had a good linearity in the ranges of 0.021-0.412 μg(r=0.999 9) for mangiferin, 0.004-0.083 μg(r=0.999 0)for ferulic acid, 0.020-0.402 μg(r=0.999 9) for liquiritin and 0.019-0.348 μg(r=0.999 9) for spinosin, 0.094-1.890 μg(r=0.999 0) for timosaponin BII, 0.020-0.410 μg (r=0.999 2) for jujuboside A, 0.051-1.025 μg(r=0.999 1) for betulinic acid and 0.013-0.270 μg(r=0.999 5) for betulin. The average recovery were 103.0%, 101.2%, 102.6%, 100.6%, 100.6%, 100.7%, 98.0%, 101.2% (n=6), respectively. The contents of three batches of samples were 0.534-0.911 mg·g^-1 for mangiferin, 0.114-0.213 mg·g^-1 for ferulic acid, 0.534-0.552 mg·g^-1 for liquiritin, 0.641-0.733 mg·g^-1 for spinosin, 1.066-1.208 mg·g^-1 for timosaponin B Ⅱ, 0.644-0.845 mg·g^-1 for jujuboside A, 2.181-2.211 mg·g^-1 for betulinic acid, and 0.307-0.309 mg·g^-1 for betulin. Conclusion: This method is proved to be valid for the quality control of compound Semen Ziziphi Spinoase granules.