HPLC-PDA法同时测定大黄蛰虫丸中6种成分的含量
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摘要
目的:建立同时测定大黄蛰虫丸中苦杏仁苷、芍药苷、黄芩苷、甘草酸、大黄素及大黄酚含量的方法。方法:采用高效液相色谱法。色谱柱为Welchrom-C_(18),流动相为甲醇-0.1%磷酸(梯度洗脱),流速为1.0 mL/min,柱温为30℃,检测波长为210 nm(苦杏仁苷)、230 nm(芍药苷、黄芩苷)和250 nm[甘草酸(以甘草酸铵计)、大黄素、大黄酚],进样量为10μL。结果:苦杏仁苷、芍药苷、黄芩苷、甘草酸、大黄素及大黄酚检测质量浓度线性范围分别为21.028～157.71、12.052～90.390、34.288～257.16、8.252 0～61.890、3.272 0～24.540、4.768 0～35.760μg/mL(r均≥0.999 2);检测限分别为0.105 0、0.121 0、0.068 6、0.082 5、0.024 6、0.0179μg/m L;定量限分别为0.263 0、0.362 0、0.171 0、0.268 0、0.065 5、0.047 7μg/mL;精密度、稳定性(12 h)、重复性试验的RSD均<2.00%(n=6);加样回收率分别为96.01%～100.76%、97.09%～101.86%、99.70%～101.99%、96.29%～99.52%、98.47%～102.14%、97.19%～99.16%,RSD分别为1.63%、1.50%、0.82%、1.35%、1.35%、0.69%(n=6)。结论:该方法准确、简便、重复性好,可用于同时测定大黄蛰虫丸中苦杏仁苷、芍药苷、黄芩苷、甘草酸、大黄素及大黄酚的含量。
OBJECTIVE: To establish a method for amygdalin, paeoniforin, baicalin, glycyrrhizic acid, emodin and chrysophanol in Dahuang zhechong pills. METHODS:HPLC method was adopted. The determination was performed on Welchrom C_(18) with mobile phase consisted of methanol-0.1% phosphoric acid(gradient elution)at the flow rate of 1.0 m L/min. The column temperature was set at 30 ℃,and the detection wavelengths were set at 210 nm(amygdalin),230 nm(paeoniforin,baicalin)and250 nm [glycyrrhizic acid(calculated with ammonium glycyrrhizinate),emodin,chrysophanol]. The sample size was 10 μL.RESULTS:The linear ranges of amygdalin,paeonifiorin,baicalin,ammonium glycyrrhizinate,emodin and chrysophanol fell within the ranges of 21.028-157.71,2.052-90.390,34.288-257.16,8.252 0-61.890,3.272 0-24.540,4.768 0-35.760 μg/m L(all r≥0.999 2).The limits of detection were 0.105 0,0.121 0,0.068 6,0.082 5,0.024 6,0.017 9 μ g/m L. The limits of quantitation were0.263 0,0.362 0,0.171 0,0.268 0,0.065 5,0.047 7 μg/mL. RSDs of precision,stability(12 h)and reproducibility tests were lower than 2.00%(n=6). The average recoveries were 96.01%-100.76%(RSD=1.63%,n=6),97.09%-101.86%(RSD=1.50%,n=6),99.70%-101.99%(RSD=0.82%,n=6),96.29%-99.52%(RSD=1.35%,n=6),98.47%-102.14%(RSD=1.35%,n=6)and 97.19%-99.16%(RSD=0.69%,n=6),respectively. CONCLUSIONS:The method is accurate,simple and reproducible for simultaneous determination of amygdalin,paeoniforin,baicalin,glycyrrhizic acid,emodin and chrysophanol in Dahuang zhechong pills.
OBJECTIVE: To establish a method for amygdalin, paeoniforin, baicalin, glycyrrhizic acid, emodin and chrysophanol in Dahuang zhechong pills. METHODS:HPLC method was adopted. The determination was performed on Welchrom C_(18) with mobile phase consisted of methanol-0.1% phosphoric acid(gradient elution)at the flow rate of 1.0 m L/min. The column temperature was set at 30 ℃,and the detection wavelengths were set at 210 nm(amygdalin),230 nm(paeoniforin,baicalin)and250 nm [glycyrrhizic acid(calculated with ammonium glycyrrhizinate),emodin,chrysophanol]. The sample size was 10 μL.RESULTS:The linear ranges of amygdalin,paeonifiorin,baicalin,ammonium glycyrrhizinate,emodin and chrysophanol fell within the ranges of 21.028-157.71,2.052-90.390,34.288-257.16,8.252 0-61.890,3.272 0-24.540,4.768 0-35.760 μg/m L(all r≥0.999 2).The limits of detection were 0.105 0,0.121 0,0.068 6,0.082 5,0.024 6,0.017 9 μ g/m L. The limits of quantitation were0.263 0,0.362 0,0.171 0,0.268 0,0.065 5,0.047 7 μg/mL. RSDs of precision,stability(12 h)and reproducibility tests were lower than 2.00%(n=6). The average recoveries were 96.01%-100.76%(RSD=1.63%,n=6),97.09%-101.86%(RSD=1.50%,n=6),99.70%-101.99%(RSD=0.82%,n=6),96.29%-99.52%(RSD=1.35%,n=6),98.47%-102.14%(RSD=1.35%,n=6)and 97.19%-99.16%(RSD=0.69%,n=6),respectively. CONCLUSIONS:The method is accurate,simple and reproducible for simultaneous determination of amygdalin,paeoniforin,baicalin,glycyrrhizic acid,emodin and chrysophanol in Dahuang zhechong pills.
引文
[1]林佑武,张诗军,陈泽雄,等.大黄蛰虫丸治疗非弥漫性脂肪肝疗效观察[J].中药材,2003,26(5):388-389.
[2]潘志恒,程木华,李林,等.大黄蛰虫丸抗肝纤维化作用的临床研究[J].中国中西医结合消化杂志,2003,11(4):212-214.
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[5]王云,张雪,麻印莲,等.熟大黄的炮制、药效及临床应用研究进展[J].中国实验方剂学杂志,2018,24(24):1-8.
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[7]张平,俞永梅,储忠英.高效液相色谱-二极管阵列法同时测定三黄血清口服液中5个成分[J].中成药,2014,36(1):94-97.
[8]郗洋,张熙洁,刘晓红.HPLC法同时测定连翘败毒丸中5种成分的含量[J].中国药房,2016,27(6):815-818.
[9]周欣,杨文业.高效液相色谱法测定丹栀逍遥丸中栀子苷、芍药苷、丹皮酚和甘草酸含量[J].药物分析杂志,2005,25(7):784-787.
[10]桂蜀华,陈军.HPLC法同时测定银翘柴桂颗粒中绿原酸、芍药苷和黄芩苷[J].中成药,2011,33(7):1175-1178.
[11]黄山君,杨琪伟,石燕红,等.一测多评法测定白芍中芍药苷与芍药内脂苷的含量[J].中国中药杂志,2011,36(6):780-783.
[12]高敏.HPLC法测定桑菊感冒颗粒中苦杏仁苷的含量[J].海峡药学,2013,25(9):59-60.
[13]冯江江.风热感冒颗粒中苦杏仁苷和绿原酸及连翘苷的多波长HPLC法含量测定[J].抗感染药学,2018,15(1):11-14.
[14]周军,张蕾,张茉,等.HPLC法同时测定香连化滞丸中7种成分的含量[J].中国药房,2016,27(6):840-843.
[15]张捷,谭生建,王欢,等.高效液相色谱法测定小儿润肺止咳口服液中橙皮苷和黄芩苷的含量[J].药物分析杂志,2010,30(8):1451-1453.
[16]唐德智.HPLC法测定复方黄芩片中6种成分的含量[J].药物分析杂志,2016,36(10):1870-1874.
[2]潘志恒,程木华,李林,等.大黄蛰虫丸抗肝纤维化作用的临床研究[J].中国中西医结合消化杂志,2003,11(4):212-214.
[3]陈开文,谭涌.大黄蛰虫丸临床应用研究进展[J].中国药业,2006,15(20):63-64.
[4]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:105.
[5]王云,张雪,麻印莲,等.熟大黄的炮制、药效及临床应用研究进展[J].中国实验方剂学杂志,2018,24(24):1-8.
[6]罗亚虹,张志军.动物类中药材质量控制研究新进展[J].海峡药学,2016,28(8):55-56.
[7]张平,俞永梅,储忠英.高效液相色谱-二极管阵列法同时测定三黄血清口服液中5个成分[J].中成药,2014,36(1):94-97.
[8]郗洋,张熙洁,刘晓红.HPLC法同时测定连翘败毒丸中5种成分的含量[J].中国药房,2016,27(6):815-818.
[9]周欣,杨文业.高效液相色谱法测定丹栀逍遥丸中栀子苷、芍药苷、丹皮酚和甘草酸含量[J].药物分析杂志,2005,25(7):784-787.
[10]桂蜀华,陈军.HPLC法同时测定银翘柴桂颗粒中绿原酸、芍药苷和黄芩苷[J].中成药,2011,33(7):1175-1178.
[11]黄山君,杨琪伟,石燕红,等.一测多评法测定白芍中芍药苷与芍药内脂苷的含量[J].中国中药杂志,2011,36(6):780-783.
[12]高敏.HPLC法测定桑菊感冒颗粒中苦杏仁苷的含量[J].海峡药学,2013,25(9):59-60.
[13]冯江江.风热感冒颗粒中苦杏仁苷和绿原酸及连翘苷的多波长HPLC法含量测定[J].抗感染药学,2018,15(1):11-14.
[14]周军,张蕾,张茉,等.HPLC法同时测定香连化滞丸中7种成分的含量[J].中国药房,2016,27(6):840-843.
[15]张捷,谭生建,王欢,等.高效液相色谱法测定小儿润肺止咳口服液中橙皮苷和黄芩苷的含量[J].药物分析杂志,2010,30(8):1451-1453.
[16]唐德智.HPLC法测定复方黄芩片中6种成分的含量[J].药物分析杂志,2016,36(10):1870-1874.