多波长HPLC法测定加味逍遥丸中多种成分含量及化学计量学分析
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摘要
目的:建立多指标含量测定结合化学计量学分析法,评价加味逍遥丸质量。方法:样品经甲醇超声提取,采用Kromasil C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.2%磷酸水溶液进行梯度洗脱,234nm和440 nm双波长检测,并使用雷达图分析、聚类热图分析和夹角余弦相似度分析方法对数据进行统计。结果:样品中芍药苷、丹皮酚、阿魏酸、甘草苷、甘草酸、栀子苷、西红花苷Ⅰ和西红花苷Ⅱ的含量分别为1.484~5.508、0.94~3.28、0.014~0.147、0.23~1.79、0.353~2.488、2.40~11.33、0.008 6~0.731 1和0.001 6~0.072 3 mg·g~(-1)。化学计量学分析表明各厂家的样品间存在一定差异,同一厂家的样品较为一致。区分各类样品的强特征峰为栀子苷峰、芍药苷峰、丹皮酚峰、栀子peak 6、甘草苷峰、西红花苷Ⅰ峰和牡丹皮peak2。结论:该法准确、专属,适用于加味逍遥丸整体质量评价。
Objective:To establish a method for overall quality evaluation of Jiawei Xiaoyao pills by multicomponent determination and chemometric analysis.Methods:The samples were extracted by ultrasonic with methanol.Separation was performed on a Kromasil ODS column(250 mm×4.6 mm,5μm)with a gradient elution of acetonitrile and 0.2%phosphoric acid.The detection wavelength was at 234 nm and 440 nm.The radar chart,HCA heatmap and cosine similarity were used for data analysis.Results:The content of paeoniflorin,paeonol,ferulic acid,liquiritin,glycyrrhizic acid,geniposide,crocinⅠand crocinⅡwere 1.484-5.508 mg·g~(-1),0.94-3.28 mg·g~(-1),0.014-0.147 mg·g~(-1),0.23-1.79 mg·g~(-1),0.353-2.488 mg·g~(-1),2.40-11.33 mg·g~(-1),0.008 6-0.731 1 mg·g~(-1)and 0.001 6-0.072 3 mg·g~(-1),respectively.Chemometric analysis showed that there were some differences among the samples from different manufacturers,and the samples from the same manufacturer were more consistent.Strong characteristic peaks for discrimination of different samples were geniposide peak,paeoniflorin peak,paeonol peak,peak 6 of Gardeniae Fructus,liquiritin peak,crocinⅠpeak and peak 2 of Moutan Cortex.Conclusion:The method is accurate and specific,which can be used for overall quality evaluation of Jiawei Xiaoyao pills.
Objective:To establish a method for overall quality evaluation of Jiawei Xiaoyao pills by multicomponent determination and chemometric analysis.Methods:The samples were extracted by ultrasonic with methanol.Separation was performed on a Kromasil ODS column(250 mm×4.6 mm,5μm)with a gradient elution of acetonitrile and 0.2%phosphoric acid.The detection wavelength was at 234 nm and 440 nm.The radar chart,HCA heatmap and cosine similarity were used for data analysis.Results:The content of paeoniflorin,paeonol,ferulic acid,liquiritin,glycyrrhizic acid,geniposide,crocinⅠand crocinⅡwere 1.484-5.508 mg·g~(-1),0.94-3.28 mg·g~(-1),0.014-0.147 mg·g~(-1),0.23-1.79 mg·g~(-1),0.353-2.488 mg·g~(-1),2.40-11.33 mg·g~(-1),0.008 6-0.731 1 mg·g~(-1)and 0.001 6-0.072 3 mg·g~(-1),respectively.Chemometric analysis showed that there were some differences among the samples from different manufacturers,and the samples from the same manufacturer were more consistent.Strong characteristic peaks for discrimination of different samples were geniposide peak,paeoniflorin peak,paeonol peak,peak 6 of Gardeniae Fructus,liquiritin peak,crocinⅠpeak and peak 2 of Moutan Cortex.Conclusion:The method is accurate and specific,which can be used for overall quality evaluation of Jiawei Xiaoyao pills.
引文
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[8]杨庆胜,冯朝岭,司根令.HPLC同时测定加味逍遥丸中栀子苷和芍药苷的含量[J].中国现代中药,2015,17(1):61YANG QS,FENG CL,SI GL.Determination of geniposide and paeoniflorin in Jiaweixiaoyao pills by HPLC[J].Mod Chin Med,2015,17(1):61
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[10]陈帅,王磊,高双,等.HPLC-DAD法同时测定加味逍遥丸中8种成分[J].中草药,2016,47(21):3829CHEN S,WANG L,GAO S,et al.Simultaneous determination of eight components in Jiawei Xiaoyao pills by HPLC-DAD[J].Chin Tradit Herb Drugs,2016,47(21):3829
[11]QIN F,HUANG J,QIU X,et al.Quality control of modified Xiaoyao San through the determination of 22 active components by ultra-performance liquid chromatography[J].J AOAC Int,2011,94(6):1778
[12]李明月,周立红,章顺楠,等.加味逍遥提取物超高效液相色谱指纹图谱研究[J].药物评价研究,2016,39(2):230LI MY,ZHOU LH,ZHANG SN,et al.UPLC fingerprint of extract of modified Xiaoyao[J].Drug Eval Res,2016,39(2):230
[13]王赵,陈玉武,王琼,等.硫熏白芍的质量评价[J].中国中药杂志,2014,16(8):3074WANG Z,CHEN YW,WANG Q,et al.Quality assessment of sulfur-fumigated Paeoniae Alba Radix[J].China J Chin Mater Med,2014,16(8):3074
[14]孙国祥,侯志飞,张春玲,等.色谱指纹图谱定性相似度和定量相似度的比较研究[J].药学学报,2007,42(1):75SUN GX,HOU ZF,ZHANG CL,et al.Comparison between the qualitative similarity and the quantitative similarity of chromatographic fingerprints of traditional Chinese medicines[J].Acta Pharm Sin,2007,42(1):75
[15]孙国祥,宋杨,毕雨萌,等.色谱指纹图谱全定性相似度和全定量相似度质控体系研究[J].中南药学,2007,5(3):263SUN GX,SONG Y,BI YM,et al.Quality control system of overall qualitative similarities and overall quantitative similarities of chromatographic fingerprints[J].Cent South Pharm,2007,5(3):263
[16]孙国祥,任培培,毕雨萌,等.双定性双定量相似度法评价银杏达莫注射液的高效液相色谱指纹图谱[J].色谱,2007,25(4):518SUN GX,REN PP,BI YM,et al.Quality assessment of high performance liquid chromatographic fingerprints of Ginkgo leaf extract and dipyridamole injection by double qualitative similarities and double quantitative similarities[J].Chin J Chromatogr,2007,25(4):518
[2]张庆,沈美琼.HPLC法测定加味逍遥丸中芍药苷的含量[J].中国药师,2009,12(4):468ZHANG Q,SHEN MQ.Determination of paeoniflorin in Jiaweixiaoyao pills by HPLC[J].China Pharm,2009,12(4):468
[3]李珂,贾宝秀,刘彩红,等.高效液相色谱法测定加味逍遥丸中丹皮酚的含量[J].医药导报,2010,29(10):1354LI K,JIA BX,LIU CH,et al.Determination of paeonol in Jiaweixiaoyao pills by HPLC[J].Her Med,2010,29(10):1354
[4]任红心.RP-HPLC法测定加味逍遥丸中栀子苷的含量[J].中医研究,2012,25(5):71REN HX.Determination of geniposide in Jiaweixiaoyao pills by RP-HPLC[J].Tradit Chin Med Res,2012,25(5):71
[5]陈玉杰.高效毛细管电泳法测定加味逍遥丸中芍药苷、栀子苷的含量[J].中国实验方剂学杂志,2012,18(10):146CHEN YJ.Determination of paeoniflorin and geniposide in Jiawei Xiaoyao pills by high performance capillary electrophoresis[J].Chin J Exp Tradit Med Form,2012,18(10):146
[6]魏龙.高效液相色谱法测定加味逍遥丸芍药苷的含量[J].中国医药指南,2013,11(29):47WEI L.Determination of paeoniflorin in Jiaweixiaoyao pills by HPLC[J].Guide China Med,2013,11(29):47
[7]杜蓉,张孟佑.HPLC法测定加味逍遥丸中芍药苷与甘草苷的含量[J].中国药房,2015,26(18):2571DU R,ZHANG MY.Content determination of paeoniflorin and liquoritin in Jiaweixiaoyao pills by HPLC[J].China Pharm,2015,26(18):2571
[8]杨庆胜,冯朝岭,司根令.HPLC同时测定加味逍遥丸中栀子苷和芍药苷的含量[J].中国现代中药,2015,17(1):61YANG QS,FENG CL,SI GL.Determination of geniposide and paeoniflorin in Jiaweixiaoyao pills by HPLC[J].Mod Chin Med,2015,17(1):61
[9]钱鑫,徐飞.高效液相色谱法测定加味逍遥丸中甘草酸[J].现代药物与临床,2013,28(2):194QIAN X,XU F.Determination of glycyrrhizic acid in Jiawei Xiaoyao pills by HPLC[J].Drugs Clin,2013,28(2):194
[10]陈帅,王磊,高双,等.HPLC-DAD法同时测定加味逍遥丸中8种成分[J].中草药,2016,47(21):3829CHEN S,WANG L,GAO S,et al.Simultaneous determination of eight components in Jiawei Xiaoyao pills by HPLC-DAD[J].Chin Tradit Herb Drugs,2016,47(21):3829
[11]QIN F,HUANG J,QIU X,et al.Quality control of modified Xiaoyao San through the determination of 22 active components by ultra-performance liquid chromatography[J].J AOAC Int,2011,94(6):1778
[12]李明月,周立红,章顺楠,等.加味逍遥提取物超高效液相色谱指纹图谱研究[J].药物评价研究,2016,39(2):230LI MY,ZHOU LH,ZHANG SN,et al.UPLC fingerprint of extract of modified Xiaoyao[J].Drug Eval Res,2016,39(2):230
[13]王赵,陈玉武,王琼,等.硫熏白芍的质量评价[J].中国中药杂志,2014,16(8):3074WANG Z,CHEN YW,WANG Q,et al.Quality assessment of sulfur-fumigated Paeoniae Alba Radix[J].China J Chin Mater Med,2014,16(8):3074
[14]孙国祥,侯志飞,张春玲,等.色谱指纹图谱定性相似度和定量相似度的比较研究[J].药学学报,2007,42(1):75SUN GX,HOU ZF,ZHANG CL,et al.Comparison between the qualitative similarity and the quantitative similarity of chromatographic fingerprints of traditional Chinese medicines[J].Acta Pharm Sin,2007,42(1):75
[15]孙国祥,宋杨,毕雨萌,等.色谱指纹图谱全定性相似度和全定量相似度质控体系研究[J].中南药学,2007,5(3):263SUN GX,SONG Y,BI YM,et al.Quality control system of overall qualitative similarities and overall quantitative similarities of chromatographic fingerprints[J].Cent South Pharm,2007,5(3):263
[16]孙国祥,任培培,毕雨萌,等.双定性双定量相似度法评价银杏达莫注射液的高效液相色谱指纹图谱[J].色谱,2007,25(4):518SUN GX,REN PP,BI YM,et al.Quality assessment of high performance liquid chromatographic fingerprints of Ginkgo leaf extract and dipyridamole injection by double qualitative similarities and double quantitative similarities[J].Chin J Chromatogr,2007,25(4):518