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刊物信息
期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
编辑部主任:粟晓黎
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237

 

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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

Simultaneous determination of eight active components in compound Semen Ziziphi Spinoase granules by UPLC-DAD-ELSD wavelength switching

分类号:
出版年·卷·期(页码):2016,36 (10):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

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