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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BⅡ、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,1.8μm),流动相为乙腈-0.1%醋酸溶液,梯度洗脱,流速0.4mL·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-BⅡ、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BⅡ、酸枣仁皂苷A、白桦脂酸、白桦脂醇的进样量分别在0.021~0.412μg(r=0.999 9)、0.004~0.083μg(r=0.999 0)、0.020~0.402μg(r=0.999 9)、0.019~0.348μg(r=0.999 9)、0.094~1.890μg(r=0.999 0)、0.020~0.410μg(r=0.999 2)、0.051~1.025μg(r=0.999 1)和0.013~0.270μg(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·g1,斯皮诺素含量为0.641~0.733 mg·g~(-1),知母皂苷BⅡ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 UPLC-DAD-ELSD switched-wavelength method for the determination of mangiferin, ferulic acid, glycyrrhizin, spinosin, timosaponin BⅡ, jujuboside A, betulinic acid and betulin in Suanzaoren granule . Methods: The mobile phase was acetonitrile-0.1% acetic acid with a gradient of 0.4 mL · min ~ (-1) on an Agilent Zorbax Eclipse plus C18 column (2.1 mm × 50 mm, 1.8 μm) The wavelength was 250 nm (0-5.8 min, ferulic acid), 280 nm (5.8-25 min, glycyrrhizin, spinosyn) and the column temperature was 40 ℃. Evaporative light scattering detector , Jujuboside A, betulinic acid and betulin). The temperature of nebulizer was 40 ℃, the temperature of drift tube was 100 ℃ and the gas flow rate was 1.60 L · min ~ (-1). Results: The separation of the tested components was good. The injection volume of mangiferin, ferulic acid, glycyrrhizin, spinosin, timosaponin B Ⅱ, jujuboside A, betulinic acid and betulin were respectively 0.021 (R = 0.999 9), 0.019-0.348 μg (r = 0.999 9), 0.094-1.890 μg (r = 0.999 9) 0.999 0), 0.020 ~ 0.410μg (r = 0.999 2), 0.051 ~ 1.025μg (r = 0.999 1) and 0.013 ~ 0.270μg (r = 0.999 5) , The content of ferulic acid was 0.114-0.213 mg · g -1, the content of liquiritin was 0.534-0.552 mg · g -1, the content of spindolin was 0.641-0.90 mg · g -1, 0.733 mg · g ~ (-1), the content of B Ⅱ in Fructus schisandrae was 1.066 ~ 1.208 mg · g -1, the content of Jujuboside A was 0.644 ~ 0.845 mg · g -1, the content of Betulinic acid Was 2.181 ~ 2.211 mg · g -1, and the content of betulin was 0.307 ~ 0.309 mg · g -1. Conclusion: This method can be used for the quality control of Fufang Suanzaoren granules by the methodological verification.