肺抑瘤合剂质量标准研究
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摘要
目的:对肺抑瘤合剂进行薄层鉴别及定量测定,建立合理可行的质量控制方法与标准。方法:采用薄层色谱法(TLC)对制剂中黄芪、薏苡仁、浙贝母、甘草进行定性鉴别;建立测定肺抑瘤合剂中指标性成分黄芪甲苷的高效液相色谱-蒸发光散射检测(HPLC-ELSD)方法;采用Agilent ZORBAXSB-C_(18)色谱柱(4. 6 mm×250 mm,5μm),流动相为乙腈-水(32∶68),流速为1. 0 mL/min,柱温为25℃。ELSD参数:漂移管温度为90℃,雾化温度为40℃,氮气流速为1. 20 L/min。结果:TLC图斑点清晰,专属性强,能有效鉴别4味药材;黄芪甲苷进样量在0. 9160～9. 1600μg范围内与峰面积线性关系良好,回归方程为l gY=1. 418l g X+2. 480,r=0. 999 5,平均加样回收率为96. 99%,RSD为0. 96%(n=6)。结论:建立的鉴别和含量测定方法专属性强、重复性好、简便准确,可作为控制肺抑瘤合剂质量的方法。
Objective: To establish the rational and feasible method and standard of quality control by performing thin-layer chromatography(TLC) identification and quantitative determination of pulmonary tumor-inhibiting mixture. Methods: HuangQi[Astragalus membranaceus(Fisch.) Bunge.], Yiyiren(semen coicis), ZheBeiMu(Fritillaria thunbergii Miq.) and GanCao(licorice) in the preparations were identified qualitatively by TLC, and HPLC-ELSD method of indicative components Astragaloside A contained in pulmonary tumor-inhibiting mixture was established,AgilentZORBAX SB-C_(18) chromatographic column(4.6 mm×250 mm,5 μm) was used, acetonitrile-water(32:68) as mobile phase, flow velocity was 1.0 m L/min, column temperature was 25℃. ELSD parameters: the temperature of drift tube was 90℃, atomization temperature 40℃, nitrogen velocity was 1.20 L/min. Results: TLC spots were clear with strong specialization, and four kinds of herbs could be effectively identified; astragaloside A was in good linear relationship in the peak area and the range from 0.916 0 to 9.160 0 μg, regression equation was lgY=1.418 lgX+2.480, r=0.999 5, average sample recovery was 96.99%, RSD was 0.96%(n=6). Conclusion: The established identification and content determination methods, which are specific, reproducible, simple and accurate, could be taken as the method of controlling the quality of pulmonary tumor-inhibiting mixture.
Objective: To establish the rational and feasible method and standard of quality control by performing thin-layer chromatography(TLC) identification and quantitative determination of pulmonary tumor-inhibiting mixture. Methods: HuangQi[Astragalus membranaceus(Fisch.) Bunge.], Yiyiren(semen coicis), ZheBeiMu(Fritillaria thunbergii Miq.) and GanCao(licorice) in the preparations were identified qualitatively by TLC, and HPLC-ELSD method of indicative components Astragaloside A contained in pulmonary tumor-inhibiting mixture was established,AgilentZORBAX SB-C_(18) chromatographic column(4.6 mm×250 mm,5 μm) was used, acetonitrile-water(32:68) as mobile phase, flow velocity was 1.0 m L/min, column temperature was 25℃. ELSD parameters: the temperature of drift tube was 90℃, atomization temperature 40℃, nitrogen velocity was 1.20 L/min. Results: TLC spots were clear with strong specialization, and four kinds of herbs could be effectively identified; astragaloside A was in good linear relationship in the peak area and the range from 0.916 0 to 9.160 0 μg, regression equation was lgY=1.418 lgX+2.480, r=0.999 5, average sample recovery was 96.99%, RSD was 0.96%(n=6). Conclusion: The established identification and content determination methods, which are specific, reproducible, simple and accurate, could be taken as the method of controlling the quality of pulmonary tumor-inhibiting mixture.
引文
[1]国家药典委员会.中华人民共和国药典:一部[M].北京:中国医药科技出版社,2015:283.
[2]吴青业,周恩丽,付小环,等.HPLC-ELSD法测定芪葛口服液中黄芪甲苷[J].中草药,2010,41(8):1305-1306.
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[5]欧阳春华.黄芪甲苷含量测定几种常用方法的比较[J].中国现代药物应用,2009,3(15):139-141.
[6]盛家荣.HPLC测定十五味气血双补口服液中黄芪甲苷的含量[J].中成药,2006,28(11):1690-1691.
[2]吴青业,周恩丽,付小环,等.HPLC-ELSD法测定芪葛口服液中黄芪甲苷[J].中草药,2010,41(8):1305-1306.
[3]李建芳,黄劲通.参茯益气安神合剂中黄芪甲苷的含量测定[J].中国实验方剂学杂志,2014,20(9):102-104.
[4]冯传平,杨惠,狄庆锋,等.HPLC-ELSD法测定补肾温肺合剂中黄芪甲苷的含量[J].中国药师,2014,17(2):322-324.
[5]欧阳春华.黄芪甲苷含量测定几种常用方法的比较[J].中国现代药物应用,2009,3(15):139-141.
[6]盛家荣.HPLC测定十五味气血双补口服液中黄芪甲苷的含量[J].中成药,2006,28(11):1690-1691.