HPLC-DAD法同时测定宁泌泰胶囊中5个有效成分的含量
|
摘要
目的:建立HPLC法同时测定宁泌泰胶囊中没食子酸、盐酸小檗碱、连翘酯苷A、芦丁和槲皮素5个成分的含量。方法:采用Diamonsil C_(18)色谱柱(250 mm×4.6 mm,5μm),以甲醇-0.1%磷酸水为流动相,梯度洗脱,流速为1.0 mL·min~(-1),柱温为25℃,检测波长为256、280、330 nm。结果:没食子酸在0.004 9～0.121 5 mg·mL~(-1)、小檗碱在0.028 4～0.710 0 mg·mL~(-1)、连翘酯苷A在0.227 0～5.675 0 mg·mL~(-1)、芦丁在0.014 4～0.360 5 mg·mL~(-1)、槲皮素在0.062 2～1.554 0 mg·mL~(-1)浓度范围内线性关系均良好(r>0.999 5),平均加样回收率为98.1%～99.5%,RSD为0.81%～1.8%。测定宁必泰胶囊样品中没食子酸、小檗碱、连翘酯苷A、芦丁、槲皮素的平均含量分别为0.022%、0.078%、0.552%、0.040%和0.163%。结论:该方法简便准确,重复性好,可用于宁泌泰胶囊的质量控制。
Objective:To establish an HPLC method for simultaneous determination of 5 components(gallic acid,berberine hydrochloride,forsythiaside A,rutin and quercetin)in Ningmitai capsules. Methods:The separation was performed on a Diamonsil C_(18) column(250 mm×4.6 mm,5 μm),with methanol-0.1% phosphoric acid as the mobile phase in gradient elution at a flow rate of 1.0 mL·min~(-1). The column temperature was 25 ℃ and the detection wavelengths were 256,280 and 330 nm. Results:The linear relationship of gallic acid in 0.004 9-0.121 5 mg·mL~(-1), berberine at 0.028 4-0.710 0 mg·mL~(-1),forsythione A at 0.227 0-5.675 0 mg·mL~(-1),rutin at 0.014 4-0.360 5 mg·mL~(-1) and quercetin at 0.062 2-1.554 0 mg·mL~(-1) were all good(r>0.999 5). The average recoveries were 98.1%-99.5% and the RSDs were 0.81%-1.8%,respectively. The average contents of gallic acid,berberine,forsythin A,rutin and quercetin in Ningmitai capsules samples were 0.022%,0.078%,0.552%,0.040% and 0.163%,respectively. Conclusion:This method is simple,accurate and reproducible,and can be used for the quality control of Ningmitai capsules.
Objective:To establish an HPLC method for simultaneous determination of 5 components(gallic acid,berberine hydrochloride,forsythiaside A,rutin and quercetin)in Ningmitai capsules. Methods:The separation was performed on a Diamonsil C_(18) column(250 mm×4.6 mm,5 μm),with methanol-0.1% phosphoric acid as the mobile phase in gradient elution at a flow rate of 1.0 mL·min~(-1). The column temperature was 25 ℃ and the detection wavelengths were 256,280 and 330 nm. Results:The linear relationship of gallic acid in 0.004 9-0.121 5 mg·mL~(-1), berberine at 0.028 4-0.710 0 mg·mL~(-1),forsythione A at 0.227 0-5.675 0 mg·mL~(-1),rutin at 0.014 4-0.360 5 mg·mL~(-1) and quercetin at 0.062 2-1.554 0 mg·mL~(-1) were all good(r>0.999 5). The average recoveries were 98.1%-99.5% and the RSDs were 0.81%-1.8%,respectively. The average contents of gallic acid,berberine,forsythin A,rutin and quercetin in Ningmitai capsules samples were 0.022%,0.078%,0.552%,0.040% and 0.163%,respectively. Conclusion:This method is simple,accurate and reproducible,and can be used for the quality control of Ningmitai capsules.
引文
[1]窦圣姗,张飞,张杰.宁泌泰胶囊化学及药理学研究进展[J].中国中医药现代远程教育,2016,14(19):151DOU SS,ZHANG F,ZHANG J.Chemical and pharmacological research progress of Ningmitai capsule[J].Chin Med Mod Dis Educ China,2016,14(19):151
[2]胡珍真,段燕康,杨素娜,等.宁泌泰胶囊临床应用新进展[J].中国中西医结合外科杂志,2014,20(6):672HU ZZ,DUAN YK,YANG SN,et al.New progress in clinical application of Ningmitai capsule[J].Chin J Integr Tradit Chin West Med,2014,20(6):672
[3]窦圣姗,张杰,陆泉.宁泌泰胶囊治疗泌尿系感染的临床研究[J].中国中医药现代远程教育,2017,15(1):98DOU SS,ZHANG J,LU Q.Clinical study of Ningmitai capsule in the treatment of urinary tract infection[J].Chin Med Mod Dis Educ China,2017,15(1):98
[4]吕炎唏,王隶书,程东岩,等.中药头花蓼的化学成分和药理作用研究概况[J].中国药师,2017,20(10):1849LüYX,WANG LS,CHENG DY,et al.Study advances in chemical constituents and pharmacological activities of Chinese medicine Polygonum capitatum[J].China Pharm,2017,20(10):1849
[5]夏晓旦,黄婷,薛嫚,等.木芙蓉化学成分与药理作用的研究进展[J].中成药,2017,39(11):2356XIA XD,HUANG T,XUE M,et al.Advances in research on chemical constituents and pharmacological effects of cottonrose hibiscus[J].Chin Tradit Pat Med,2017,39(11):2356
[6]夏伟,董诚明,杨朝帆,等.连翘化学成分及其药理学研究进展[J].中国现代中药,2016,18(12):1670XIA W,DONG CM,YANG CF,et al.Research progress on chemical constituents and pharmacology of Forsythia suspensa[J].Mod Chin Med,2016,18(12):1670
[7]徐婵,吴潇潇,万定荣,等.三颗针抗菌活性成分研究[J].华中科技大学学报(医学版),2015,44(5):556XU C,W XX,WAN DR,et al.Analysis of antimicrobial activity constituents of“San Ke Zhen”[J].Acta Med Univ Sci Technol Huazhong,2015,44(5):556
[8]成志俊.HPLC法测定宁泌泰胶囊中盐酸小檗碱的含量[J].海峡药学,2013,25(4):45.CHENG ZJ.Determination of berberine hydrochloride in Ninmitai capsules by HPLC[J].Strait Pharm J,2013,25(4):45
[9]钱淑琴,陈宗良.HPLC法测定宁泌泰胶囊中连翘苷的含量[J].中华中医药学刊,2011,29(1):208QIAN SQ,CHEN ZL.HPLC determination of forsythin in Ningmitai capsules[J].Chin Arch Tradit Chin Med,2011,29(1):208
[10]胡慧玲,沈慎,付超美,等.宁泌泰片质量标准研究[J].四川省卫生管理干部学院学报,2008(1):1HU HL,SHEN C,FU CM,et al.Study on quality standard of Ningmitai tablets[J].J Sichuan Contin Educ Coll Med Sci,2008(1):1
[11]郝乘仪,郭淑英,冯波.HPLC同时测定芎菊上清片中5种成分的含量[J].中国实验方剂学杂志,2014,20(24):74HAO CY,GUO SY,FENG B.Simultaneous determination of five compounds in Xiongju Shangqing tablets by HPLC[J].Chin J Exp Tradit Med Form,2014,20(24):74
[12]彭亮,李诒光,陈杰,等.HPLC同时测定不同产地猴耳环叶中没食子酸和槲皮素的含量[J].中国实验方剂学杂志,2015,21(11):77PENG L,LI YG,CHEN J,et al.HPLC determination of gallic acid and quercetin in Archidendri Folium from different producing areas[J].Chin J Exp Tradit Med Form,2015,21(11):77
[13]魏悦,李晓,李自红,等.HPLC同时测定连翘药材及提取物中芦丁、连翘酯苷A和连翘苷的含量[J].中国实验方剂学杂志,2013,19(9):108WEI Y,LI X,LI ZH,et al.Simultaneous determination of rutin,forsythoside A and phillyrin of Forsythiae Fructus and its extract by HPLC[J].Chin J Exp Tradit Med Form,2013,19(9):108
[2]胡珍真,段燕康,杨素娜,等.宁泌泰胶囊临床应用新进展[J].中国中西医结合外科杂志,2014,20(6):672HU ZZ,DUAN YK,YANG SN,et al.New progress in clinical application of Ningmitai capsule[J].Chin J Integr Tradit Chin West Med,2014,20(6):672
[3]窦圣姗,张杰,陆泉.宁泌泰胶囊治疗泌尿系感染的临床研究[J].中国中医药现代远程教育,2017,15(1):98DOU SS,ZHANG J,LU Q.Clinical study of Ningmitai capsule in the treatment of urinary tract infection[J].Chin Med Mod Dis Educ China,2017,15(1):98
[4]吕炎唏,王隶书,程东岩,等.中药头花蓼的化学成分和药理作用研究概况[J].中国药师,2017,20(10):1849LüYX,WANG LS,CHENG DY,et al.Study advances in chemical constituents and pharmacological activities of Chinese medicine Polygonum capitatum[J].China Pharm,2017,20(10):1849
[5]夏晓旦,黄婷,薛嫚,等.木芙蓉化学成分与药理作用的研究进展[J].中成药,2017,39(11):2356XIA XD,HUANG T,XUE M,et al.Advances in research on chemical constituents and pharmacological effects of cottonrose hibiscus[J].Chin Tradit Pat Med,2017,39(11):2356
[6]夏伟,董诚明,杨朝帆,等.连翘化学成分及其药理学研究进展[J].中国现代中药,2016,18(12):1670XIA W,DONG CM,YANG CF,et al.Research progress on chemical constituents and pharmacology of Forsythia suspensa[J].Mod Chin Med,2016,18(12):1670
[7]徐婵,吴潇潇,万定荣,等.三颗针抗菌活性成分研究[J].华中科技大学学报(医学版),2015,44(5):556XU C,W XX,WAN DR,et al.Analysis of antimicrobial activity constituents of“San Ke Zhen”[J].Acta Med Univ Sci Technol Huazhong,2015,44(5):556
[8]成志俊.HPLC法测定宁泌泰胶囊中盐酸小檗碱的含量[J].海峡药学,2013,25(4):45.CHENG ZJ.Determination of berberine hydrochloride in Ninmitai capsules by HPLC[J].Strait Pharm J,2013,25(4):45
[9]钱淑琴,陈宗良.HPLC法测定宁泌泰胶囊中连翘苷的含量[J].中华中医药学刊,2011,29(1):208QIAN SQ,CHEN ZL.HPLC determination of forsythin in Ningmitai capsules[J].Chin Arch Tradit Chin Med,2011,29(1):208
[10]胡慧玲,沈慎,付超美,等.宁泌泰片质量标准研究[J].四川省卫生管理干部学院学报,2008(1):1HU HL,SHEN C,FU CM,et al.Study on quality standard of Ningmitai tablets[J].J Sichuan Contin Educ Coll Med Sci,2008(1):1
[11]郝乘仪,郭淑英,冯波.HPLC同时测定芎菊上清片中5种成分的含量[J].中国实验方剂学杂志,2014,20(24):74HAO CY,GUO SY,FENG B.Simultaneous determination of five compounds in Xiongju Shangqing tablets by HPLC[J].Chin J Exp Tradit Med Form,2014,20(24):74
[12]彭亮,李诒光,陈杰,等.HPLC同时测定不同产地猴耳环叶中没食子酸和槲皮素的含量[J].中国实验方剂学杂志,2015,21(11):77PENG L,LI YG,CHEN J,et al.HPLC determination of gallic acid and quercetin in Archidendri Folium from different producing areas[J].Chin J Exp Tradit Med Form,2015,21(11):77
[13]魏悦,李晓,李自红,等.HPLC同时测定连翘药材及提取物中芦丁、连翘酯苷A和连翘苷的含量[J].中国实验方剂学杂志,2013,19(9):108WEI Y,LI X,LI ZH,et al.Simultaneous determination of rutin,forsythoside A and phillyrin of Forsythiae Fructus and its extract by HPLC[J].Chin J Exp Tradit Med Form,2013,19(9):108