藿芪灌注液质量标准研究
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摘要
目的建立藿芪灌注液质量标准.方法采用薄层色谱法对处方中淫羊藿、红花、丹参与益母草进行TLC定性鉴别;使用WondaSil C18柱(4.6mm×250mm,5μm),流动相∶乙腈-水(28∶72),柱温40℃,检测波长270nm,进样量10μL,流速1.0mL/min测定淫羊藿苷的含量;使用ZORBAX SB-C18柱(4.6mm×150mm,5μm),漂移管温度为90℃,载气流速为2.5L/min,流动相∶甲醇-水(65∶35),柱温40℃,流速1mL/min,用蒸发光散射检测器测定黄芪甲苷的含量.结果 TLC鉴别色谱图分离效果好,阴性对照无干扰,专属性强,重复性好;测定淫羊藿苷与黄芪甲苷含量表明,分别在2.336~58.4μg/mL(r=0.999 9)和0.047 8~0.478mg/mL(r=0.999 6)范围内与峰面积成较好的线性关系;其平均加样回收率分别为100.2%,RSD=0.45%和99.26%,RSD=1.46%.结论所建立的特征图谱专属性强、准确可行、简便、可快速用于定性鉴别、定量检测,可有效地用于该制剂的质量控制方法.
Objective To establish the quality standard for Huoqi perfusion.Methods TLC was used for qualitative identification of Epimedium,Carthamus tinctorius,Salvia miltiorrhiza and Leonuri herba.The separation of icariin was achieved by a WondaSil-C18 column(4.6 mm×250 mm,5μm),with a mobile phase composed of acetonitrile-water(28∶72),a detection wavelength of 270 nm,a column temperature of 40 ℃.an injection volume of 10μL and a flow rate of 1.0 mL/min.The separation of the astragaloside was achieved by a ZORBAX SB-C18 column(4.6 mm×150 mm,5μm)with a drift tube temperature of 90 ℃,a carrier gas flow rate of 2.5 L/min and a mobile phase composed of methanol-water(65∶35).The flow rate was 1.0 mL/min and the column temperature was 40 ℃,with an evaporative light scattering detector.Results The spots on TLC plates were clear without interference by the blank reference and with good specificity and repeatability.The linear ranges of icariin and astragaloside were obtained between2.336-58.4μg/mL(r=0.999 97)and 0.047 8-0.478 mg/mL(r=0.999 6),the recovery averaging100.2%(RSD =0.45%)and 99.26%(RSD =1.46%),respectively.Conclusion The determination method reported in this paper is specific,accurate,feasible,simple and convenient,and can be used for the determination of the active ingredients of the preparation,which provides a reference value for the quality standard of the preparation.
Objective To establish the quality standard for Huoqi perfusion.Methods TLC was used for qualitative identification of Epimedium,Carthamus tinctorius,Salvia miltiorrhiza and Leonuri herba.The separation of icariin was achieved by a WondaSil-C18 column(4.6 mm×250 mm,5μm),with a mobile phase composed of acetonitrile-water(28∶72),a detection wavelength of 270 nm,a column temperature of 40 ℃.an injection volume of 10μL and a flow rate of 1.0 mL/min.The separation of the astragaloside was achieved by a ZORBAX SB-C18 column(4.6 mm×150 mm,5μm)with a drift tube temperature of 90 ℃,a carrier gas flow rate of 2.5 L/min and a mobile phase composed of methanol-water(65∶35).The flow rate was 1.0 mL/min and the column temperature was 40 ℃,with an evaporative light scattering detector.Results The spots on TLC plates were clear without interference by the blank reference and with good specificity and repeatability.The linear ranges of icariin and astragaloside were obtained between2.336-58.4μg/mL(r=0.999 97)and 0.047 8-0.478 mg/mL(r=0.999 6),the recovery averaging100.2%(RSD =0.45%)and 99.26%(RSD =1.46%),respectively.Conclusion The determination method reported in this paper is specific,accurate,feasible,simple and convenient,and can be used for the determination of the active ingredients of the preparation,which provides a reference value for the quality standard of the preparation.
引文
[1]李世宏,严作廷,王东升,等.纯中药催情助孕液治疗奶牛卵巢性不孕症试验[J].中兽医医药杂志,2010,25(6):52-53.
[2]王东升,张世栋,李世宏,等.正交试验法优化催情助孕液制备工艺[J].中国农学通报,2012,28(29):75-78.
[3]王东升,张世栋,苗小楼,等.藿芪灌注液局部刺激性试验[J].江苏农业科学,2016,44(4):303-305.
[4]张世栋,王旭荣,杨峰,等.催情助孕液对小鼠雌、孕激素水平及其受体mRNA表达的影响[J].中国兽医学报,2013,33(7):1127-1131.
[5]国家药典委员会.中国药典2015版一部[M].北京:中国医药科技出版社,2015.
[6]HAN S,XIE Y Y,WANG Y M,et al.Comparative Study on Chemical Quality of Main Species of Epimedium[J].YaoXue XueBao,2012,47(4):502-507.
[7]俞吉,朱瑞,董妍君,等.骨疏灵颗粒不同配伍对淫羊藿苷含量的影响[J].中国药房,2016,27(1):79-81.
[8]张军,林传俊.淫羊藿苷的高效液相色谱检测方法探讨[J].时珍国医国药,2011,22(12):3027-3028.
[9]DING F F,DENG Y R,ZHANG X J,et al.Simultaneous Determination of Five Astragalosides in Astragali Radix and Jinqi Jiangtang Tablet by HPLC-ELSD[J].Journal of Chinese Medicinal Materials,2015,38(1):156.
[10]刘源焕,农毅清,陈洪涛,等.无糖型扶芳参芪口服液质量标准研究[J].时珍国医国药,2014,25(12):2912-2914.
[11]徐作刚,段萍,茅向军,等.金乌骨通胶囊HPLC指纹图谱研究[J].中国民族民间医药,2014,23(22):8-10.
[12]韩宵,朱磊,闫春风,等.HPLC-ELSD法测定益心舒片中黄芪甲苷含量[J].亚太传统医药,2016,12(1):35-37.
[13]SU B R,DENG H M,MA H L,et al.Quality Evaluation of Astragali Radix Through Chemical Pattern Recognition of Fingerprint by HPLC-dAD-ELSD[J].China Journal of Chinese Materia Medica,2013,38(19):3319-3323.
[14]CHEN H,ZHOU X,ZHAO Y,et al.HPLC-DAD-ELSD Combined Pharmacodynamics and Serum Medicinal Chemistry for Quality Assessment of Huangqi Granule[J].PLOS ONE,2015,10(4):1524-1529.
[15]PEI C,WANG Z,JIMING J A,et al.Determination of Astragaloside IVof Eight area in Astragali Radix is by HPLCELSD Internal Standard Method[J].China Journal of Chinese Materia Medica,2011,36(14):986-990.
[16]杨洪早,苗小楼,张世栋,等.藿芪灌注液中淫羊藿苷和黄芪甲苷稳定性试验研究[J].中国兽药杂志,2017,53(1):19-24.
[17]吴佳,张正锋,胡娟娟.HPLC-ELSD法同时测定参芪颗粒中6个成分的含量[J].药物分析杂志,2016,36(1):68-73.
[18]苗小楼,王东升,张世栋,等.丹翘灌注液中连翘苷的含量测定[J].中兽医医药杂志,2013,34(6):45-46.
[19]白荣,龚小倩,邱海蕴,等.反相高效液相色谱法测定心脉康合剂中淫羊藿苷含量[J].中国药业,2015,24(24):158-160.
[20]吴春丽,覃春菀,张俊霞,等.菌渣中截短侧耳素含量的高效液相色谱法测定[J].郑州大学学报(医学版),2009,44(1):178-180.
[21]MU Lu-xia,ZHU L,ZHAO A H,et al.Study on Extraction and Purification of Polysaccharides from Astragalus Membranaceus[J].Journal of Chinese Medicinal Materials,2009,32(11):15-21.
[22]XIA G P,LIU P,HAN Y M.Determination of the Total Content of Astragaloside IV in Radix Astragali[J].Journal of Chinese Medicinal Materials,2008,31(3):66-72.
[23]梁慧敏,欧妮.高效液相色谱-电喷雾检测器法测定贞芪扶正颗粒中黄芪甲苷含量[J].中国药业,2016,25(5):55-56.
[24]王东升,严作廷,李世宏,等.中兽药成方制剂质量控制的思考[J].动物医学进展,2008,13(2):109-111.
[25]王东升,尚小飞,苗小楼,等.产复康中5种中药的薄层色谱鉴别[J].黑龙江畜牧兽医,2015,19(3):155-157.
[26]苏强,倪艳,王瑞明,等.祛斑洁颜胶囊的薄层鉴别和黄芩苷的含量测定[J].中成药,2003,25(1):30-32.
[27]吴宁,胡俊杰,郑国华,等.益母妇宁胶囊的薄层色谱鉴别[J].时珍国医国药,2015,26(1):121-125.
[28]贾永艳,陈波,田效志,等.产妇康颗粒质量标准研究[J].中医学报,2013,28(3):382-384.
[29]秦永平,毛兴荣,梁茂植,等.RP-HPLC测定产妇安口服液中水苏碱的含量[J].华西药学杂志,2003,18(4):288-290.
[30]王秋珍.益母草颗粒的质量控制研究[D].广州:暨南大学,2013.
[2]王东升,张世栋,李世宏,等.正交试验法优化催情助孕液制备工艺[J].中国农学通报,2012,28(29):75-78.
[3]王东升,张世栋,苗小楼,等.藿芪灌注液局部刺激性试验[J].江苏农业科学,2016,44(4):303-305.
[4]张世栋,王旭荣,杨峰,等.催情助孕液对小鼠雌、孕激素水平及其受体mRNA表达的影响[J].中国兽医学报,2013,33(7):1127-1131.
[5]国家药典委员会.中国药典2015版一部[M].北京:中国医药科技出版社,2015.
[6]HAN S,XIE Y Y,WANG Y M,et al.Comparative Study on Chemical Quality of Main Species of Epimedium[J].YaoXue XueBao,2012,47(4):502-507.
[7]俞吉,朱瑞,董妍君,等.骨疏灵颗粒不同配伍对淫羊藿苷含量的影响[J].中国药房,2016,27(1):79-81.
[8]张军,林传俊.淫羊藿苷的高效液相色谱检测方法探讨[J].时珍国医国药,2011,22(12):3027-3028.
[9]DING F F,DENG Y R,ZHANG X J,et al.Simultaneous Determination of Five Astragalosides in Astragali Radix and Jinqi Jiangtang Tablet by HPLC-ELSD[J].Journal of Chinese Medicinal Materials,2015,38(1):156.
[10]刘源焕,农毅清,陈洪涛,等.无糖型扶芳参芪口服液质量标准研究[J].时珍国医国药,2014,25(12):2912-2914.
[11]徐作刚,段萍,茅向军,等.金乌骨通胶囊HPLC指纹图谱研究[J].中国民族民间医药,2014,23(22):8-10.
[12]韩宵,朱磊,闫春风,等.HPLC-ELSD法测定益心舒片中黄芪甲苷含量[J].亚太传统医药,2016,12(1):35-37.
[13]SU B R,DENG H M,MA H L,et al.Quality Evaluation of Astragali Radix Through Chemical Pattern Recognition of Fingerprint by HPLC-dAD-ELSD[J].China Journal of Chinese Materia Medica,2013,38(19):3319-3323.
[14]CHEN H,ZHOU X,ZHAO Y,et al.HPLC-DAD-ELSD Combined Pharmacodynamics and Serum Medicinal Chemistry for Quality Assessment of Huangqi Granule[J].PLOS ONE,2015,10(4):1524-1529.
[15]PEI C,WANG Z,JIMING J A,et al.Determination of Astragaloside IVof Eight area in Astragali Radix is by HPLCELSD Internal Standard Method[J].China Journal of Chinese Materia Medica,2011,36(14):986-990.
[16]杨洪早,苗小楼,张世栋,等.藿芪灌注液中淫羊藿苷和黄芪甲苷稳定性试验研究[J].中国兽药杂志,2017,53(1):19-24.
[17]吴佳,张正锋,胡娟娟.HPLC-ELSD法同时测定参芪颗粒中6个成分的含量[J].药物分析杂志,2016,36(1):68-73.
[18]苗小楼,王东升,张世栋,等.丹翘灌注液中连翘苷的含量测定[J].中兽医医药杂志,2013,34(6):45-46.
[19]白荣,龚小倩,邱海蕴,等.反相高效液相色谱法测定心脉康合剂中淫羊藿苷含量[J].中国药业,2015,24(24):158-160.
[20]吴春丽,覃春菀,张俊霞,等.菌渣中截短侧耳素含量的高效液相色谱法测定[J].郑州大学学报(医学版),2009,44(1):178-180.
[21]MU Lu-xia,ZHU L,ZHAO A H,et al.Study on Extraction and Purification of Polysaccharides from Astragalus Membranaceus[J].Journal of Chinese Medicinal Materials,2009,32(11):15-21.
[22]XIA G P,LIU P,HAN Y M.Determination of the Total Content of Astragaloside IV in Radix Astragali[J].Journal of Chinese Medicinal Materials,2008,31(3):66-72.
[23]梁慧敏,欧妮.高效液相色谱-电喷雾检测器法测定贞芪扶正颗粒中黄芪甲苷含量[J].中国药业,2016,25(5):55-56.
[24]王东升,严作廷,李世宏,等.中兽药成方制剂质量控制的思考[J].动物医学进展,2008,13(2):109-111.
[25]王东升,尚小飞,苗小楼,等.产复康中5种中药的薄层色谱鉴别[J].黑龙江畜牧兽医,2015,19(3):155-157.
[26]苏强,倪艳,王瑞明,等.祛斑洁颜胶囊的薄层鉴别和黄芩苷的含量测定[J].中成药,2003,25(1):30-32.
[27]吴宁,胡俊杰,郑国华,等.益母妇宁胶囊的薄层色谱鉴别[J].时珍国医国药,2015,26(1):121-125.
[28]贾永艳,陈波,田效志,等.产妇康颗粒质量标准研究[J].中医学报,2013,28(3):382-384.
[29]秦永平,毛兴荣,梁茂植,等.RP-HPLC测定产妇安口服液中水苏碱的含量[J].华西药学杂志,2003,18(4):288-290.
[30]王秋珍.益母草颗粒的质量控制研究[D].广州:暨南大学,2013.