液相色谱-质谱联用同时测定宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的含量
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摘要
目的:建立宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的含量测定方法。方法:采用Agilent Eclipse XDB-C_(18)色谱柱(150 mm×2.1 mm,5.0μm),流动相A为0.1%甲酸-10%甲醇,B为甲醇,梯度洗脱,流速为0.6 m L·min~(-1);进样量10μL,柱温30℃;采用电喷雾离子源(ESI)、正、负离子模式监测,多反应监测模式用于定量分析,喷雾电压-4.0 kV,干燥气温度为350℃,干燥气流量为11 L·min~(-1),雾化器压力为0.31 MPa。结果:没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷分别在500.0~5 000、51.00~510.0、9.000~90.00、1 034~10 340 ng·mL~(-1)内与峰面积呈良好线性关系。宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的平均加样回收率在97%~100%之间。3批宁泌泰胶囊中没食子酸、盐酸小檗碱、盐酸巴马汀、连翘苷的含量分别为3.43~4.13、0.255~0.649、0.033 8~0.068 7、2.26~3.59 mg·g~(-1)。结论:经方法学验证,本方法简单、快速、灵敏,重复性好,可以用于宁泌泰胶囊的含量测定。
Objective:To develop a method for determination of gallic acid,berberine hydrochloride,palmatine hydrochloride,forsyth in Ningmitai capsules.Methods:Analysis was performed on an Agilent Eclipse XDB-C_(18)(150 mm×2.1 mm,5.0 μm)with a gradient elution.The mobile phase consisted of 0.1% formic acid-10% methanol(A)and methanol(B)and at a flow rate of 0.6 m L·min~(-1).The injection volume was 10 μL,and the column temperature was controlled at 30 ℃.The multiple-reaction monitoring scanning was employed for the quantification with switching electrospray ion source polarity in positive and negative mode.The capillary voltage was-4.0 kV,gas temperature was 350 ℃,gas flow was 11 L·min~(-1) and nebulizer pressure was set at 0.31 MPa.Results:The linear ranges for gallic acid,berberine hydrochloride,palmatine hydrochloride,and forsyth were 500.0-5 000,51.00-510.0,9.000-90.00,and1 034-10 340 ng·mL~(-1),respectively.The recoveries were between 97%~100%.The contents of gallic acid,berberine hydrochloride,palmatine hydrochloride,and forsyth were 3.43-4.13,0.255-0.649,0.033 8-0.068 7,and 2.26-3.59 mg·g~(-1),respectively.Conclusion:The method validated was convenient,rapid,sensitive and accurate.
Objective:To develop a method for determination of gallic acid,berberine hydrochloride,palmatine hydrochloride,forsyth in Ningmitai capsules.Methods:Analysis was performed on an Agilent Eclipse XDB-C_(18)(150 mm×2.1 mm,5.0 μm)with a gradient elution.The mobile phase consisted of 0.1% formic acid-10% methanol(A)and methanol(B)and at a flow rate of 0.6 m L·min~(-1).The injection volume was 10 μL,and the column temperature was controlled at 30 ℃.The multiple-reaction monitoring scanning was employed for the quantification with switching electrospray ion source polarity in positive and negative mode.The capillary voltage was-4.0 kV,gas temperature was 350 ℃,gas flow was 11 L·min~(-1) and nebulizer pressure was set at 0.31 MPa.Results:The linear ranges for gallic acid,berberine hydrochloride,palmatine hydrochloride,and forsyth were 500.0-5 000,51.00-510.0,9.000-90.00,and1 034-10 340 ng·mL~(-1),respectively.The recoveries were between 97%~100%.The contents of gallic acid,berberine hydrochloride,palmatine hydrochloride,and forsyth were 3.43-4.13,0.255-0.649,0.033 8-0.068 7,and 2.26-3.59 mg·g~(-1),respectively.Conclusion:The method validated was convenient,rapid,sensitive and accurate.
引文
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[3]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 forsyth in Ningbitai capsules[J].Chin Arch Tradit Chin Med,2011(1):208
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[5]韦建乔.高效液相色谱/串联质谱法测定藏青果颗粒中没食子酸的含量[J].中国医院用药评价与分析,2016(S1):14WEI JQ.LC-MS/MS Determination of gallic acid in Cangqing Guo granules[J].Chin J Drug Eval Anal,2016(S1):14
[6]张晓雷,周明眉,赵爱华,等.黄连-黄芩药对化学成分的UPLCPDA-MS分析[J].天然产物研究与开发.,2012,24(11):1502ZHANG XL,ZHOU MM,ZHAO AH,et al.Analysis of the main components of coptis-scute herbal pairs by UPLC-PDA-MS[J].Nat Product Res Devel,2012,24(11):1502
[7]张艺竹,安叡,陈烨,等.LCMS/MS同时测定一清胶囊9个成分的含量[J].药物分析杂志,2013,33(7):1197ZHANG YZ,AN R,CHEN Y,et al.Simultaneous determination of nine components in Yiqing capsules by LC-MS/MS[J].Chin J Pharm Anal,2013,33(7):1197
[8]赵光,李,杜雪静.液相色谱-质谱联用法测定牡丹皮中没食子酸的含量[J].中国医学装备,2013,12(10):8ZHAO G,LI J,DU XJ.Analysis of gallic acid in Paeonia Suffruticosa andr.by HPLC-MS[J].China Med Equip,2013,12(10):8
[9]杨蓓蓓,冯茹,王维聪,等.HPLC/DAD/MS法同时测定苗药头花蓼中3种有效成分的含量[J].药物分析杂志,2008,28(11):1793YANG BB,FENG R,WANG W C,et al.Quantitative analysis of three active constituents in Miao regional herb,polygonum capitatum by HPLC/DAD/MS[J].Chin J Pharm Anal,2008,28(11):1793
[10]霍志鹏,王玉,周水平,等.黄连生物碱成分的HPLC-DAD-MS分析[J].天津药学,2016,28(2):8HUO ZP,WANG Y,ZHOU SP,et al.Analysis of main alkaloids in rhizoma coptidis by HPLC-DAD-MS[J].Tianjin Pharm,2016,28(2):8
[11]戴冬艳,朱静毅,闻琍毓.液相色谱-质谱联用技术在药物分析中的应用[J].天津药学,2012,24(3):50DAI DY,ZHU JY,WEN LY.Application of liquid chromatographymass spectrometry technology in pharmaceutical analysis[J].Tianjin Pharm,2012,24(3):50
[12]苏靖,戴荣继.液质联用技术在中药研究中的应用[J].生命科学仪器,2014,12(2):38SU J,DAI RJ.The application of liquid chromatography-mass spectrometry technology in the study of Chinese medicine[J].Life Sci Instrum,2014,12(2):38
[13]刘祥东,梁琼麟,罗国安,等.液质联用技术在医药领域中的应用[J].药物分析杂志,2005,25(1):110LIU XD,LIANG QL,LUO GA,et al.The application of liquid chromatography-mass spectrometry technology in the field of medicine[J].Chin J Pharm Anal,2005,25(1):110
[14]封美慧,邸欣,王鑫,等.RP-HPLC同时测定金银花、连翘药对提取物中6个成分的含量[J].中国实验方剂学杂志,2014,20(16):75FENG MH,DI X,WANG X,et al.Simultaneous determination of six ingredients in lonicerae japonicae flos and forsythiae fructus extracts by RP-HPLC[J].Cin J Exp Tradit Med Form,2014,20(16):75
[15]宁科贤,黄燕萍.HPLC法同时测定双黄连颗粒中绿原酸、木犀草苷、连翘苷和黄芩苷的含量[J].中国药房,2014,25(40):3819NING KX,HUANG YP.Content determination of chlorogenic acid,luteolin,forsythin and baicalin in Shuanghuanglian granules by HPLC[J].China Pharm,2014,25(40):3819
[2]成志俊.HPLC测定宁泌泰胶囊中盐酸小檗碱的含量[J].海峡药学,2013,25(4):45CHENG ZJ.Determination of berberine hydrochloride in Ningbitai capsules by HPLC[J].Strait Pharm,2013,25(4):45
[3]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 forsyth in Ningbitai capsules[J].Chin Arch Tradit Chin Med,2011(1):208
[4]曹冉冉,黄艳杰,尹卫平,等.HPLC-ESI/MS法测定不同连翘有效成分的含量[J].河南科技大学学报,2015(1):101CAO RR,HUANG YJ,YIN WP,et al.HPLC-ESI/MS determination of active constituents in forsythiae fructus of variety classes[J].J Henan Unive Sci Technol,2015,36(1):101
[5]韦建乔.高效液相色谱/串联质谱法测定藏青果颗粒中没食子酸的含量[J].中国医院用药评价与分析,2016(S1):14WEI JQ.LC-MS/MS Determination of gallic acid in Cangqing Guo granules[J].Chin J Drug Eval Anal,2016(S1):14
[6]张晓雷,周明眉,赵爱华,等.黄连-黄芩药对化学成分的UPLCPDA-MS分析[J].天然产物研究与开发.,2012,24(11):1502ZHANG XL,ZHOU MM,ZHAO AH,et al.Analysis of the main components of coptis-scute herbal pairs by UPLC-PDA-MS[J].Nat Product Res Devel,2012,24(11):1502
[7]张艺竹,安叡,陈烨,等.LCMS/MS同时测定一清胶囊9个成分的含量[J].药物分析杂志,2013,33(7):1197ZHANG YZ,AN R,CHEN Y,et al.Simultaneous determination of nine components in Yiqing capsules by LC-MS/MS[J].Chin J Pharm Anal,2013,33(7):1197
[8]赵光,李,杜雪静.液相色谱-质谱联用法测定牡丹皮中没食子酸的含量[J].中国医学装备,2013,12(10):8ZHAO G,LI J,DU XJ.Analysis of gallic acid in Paeonia Suffruticosa andr.by HPLC-MS[J].China Med Equip,2013,12(10):8
[9]杨蓓蓓,冯茹,王维聪,等.HPLC/DAD/MS法同时测定苗药头花蓼中3种有效成分的含量[J].药物分析杂志,2008,28(11):1793YANG BB,FENG R,WANG W C,et al.Quantitative analysis of three active constituents in Miao regional herb,polygonum capitatum by HPLC/DAD/MS[J].Chin J Pharm Anal,2008,28(11):1793
[10]霍志鹏,王玉,周水平,等.黄连生物碱成分的HPLC-DAD-MS分析[J].天津药学,2016,28(2):8HUO ZP,WANG Y,ZHOU SP,et al.Analysis of main alkaloids in rhizoma coptidis by HPLC-DAD-MS[J].Tianjin Pharm,2016,28(2):8
[11]戴冬艳,朱静毅,闻琍毓.液相色谱-质谱联用技术在药物分析中的应用[J].天津药学,2012,24(3):50DAI DY,ZHU JY,WEN LY.Application of liquid chromatographymass spectrometry technology in pharmaceutical analysis[J].Tianjin Pharm,2012,24(3):50
[12]苏靖,戴荣继.液质联用技术在中药研究中的应用[J].生命科学仪器,2014,12(2):38SU J,DAI RJ.The application of liquid chromatography-mass spectrometry technology in the study of Chinese medicine[J].Life Sci Instrum,2014,12(2):38
[13]刘祥东,梁琼麟,罗国安,等.液质联用技术在医药领域中的应用[J].药物分析杂志,2005,25(1):110LIU XD,LIANG QL,LUO GA,et al.The application of liquid chromatography-mass spectrometry technology in the field of medicine[J].Chin J Pharm Anal,2005,25(1):110
[14]封美慧,邸欣,王鑫,等.RP-HPLC同时测定金银花、连翘药对提取物中6个成分的含量[J].中国实验方剂学杂志,2014,20(16):75FENG MH,DI X,WANG X,et al.Simultaneous determination of six ingredients in lonicerae japonicae flos and forsythiae fructus extracts by RP-HPLC[J].Cin J Exp Tradit Med Form,2014,20(16):75
[15]宁科贤,黄燕萍.HPLC法同时测定双黄连颗粒中绿原酸、木犀草苷、连翘苷和黄芩苷的含量[J].中国药房,2014,25(40):3819NING KX,HUANG YP.Content determination of chlorogenic acid,luteolin,forsythin and baicalin in Shuanghuanglian granules by HPLC[J].China Pharm,2014,25(40):3819