UPLC法同时测定三黄睛视明丸中9个成分含量
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摘要
目的:建立超高效液相色谱法同时测定三黄睛视明丸中香蒲新苷、毛蕊异黄酮苷、异鼠李素-3-O-新橙皮苷、芒柄花苷、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1和人参皂苷Rd 9个成分的含量。方法:采用Waters Acquity UPLC?BEH C18色谱柱(2.1 mm×100 mm,1.7μm),柱温30℃,流动相为水(A)-乙腈(B),梯度洗脱,流速0.3 mL·min~(-1),检测波长203 nm。结果:香蒲新苷、毛蕊异黄酮苷、异鼠李素-3-O-新橙皮苷、芒柄花苷、三七皂苷R1、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、人参皂苷Rd的线性范围分别为1.92～36.94 ng(r=0.999 8)、1.90～36.63 ng(r=0.999 9)、1.88～36.20 ng(r=0.999 6)、0.99～19.09 ng(r=0.999 2)、40.04～770.05 ng(r=0.999 8)、107.78～2 072.68 ng(r=0.999 8)、31.74～610.34 ng(r=0.999 1)、81.33～1 564.08 ng(r=0.999 9)、19.711～379.06 ng(r=0.999 9);平均回收率(n=6)均在91%～105%之间,RSD均小于3.0%。测定的3批样品中上述9个成分含量范围分别为0.261～0.294、0.196～0.209、0.189～0.193、0.101～0.111、2.728～2.773、12.051～12.196、3.235～3.313、8.317～8.464、2.131～2.229 mg·g-1。结论:所建立的多成分含量测定方法可用于三黄睛视明丸质量控制。
Objective:To establish a UPLC method for the simultaneous determination of nine constituents in Sanhuang Jingshiming pills,including typhaneoside,calycosin-7-O-β-D-glucopyranoside,isorhamnetin-3-O-neohesperidoside,ononin,notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1,and ginsenoside Rd. Methods:The UPLC analysis was carried out by a 30 ℃ thermostatic Waters Acquity UPLC? BEH C18 column(2.1 mm×100 mm,1.7 μm) with a mobile phase composed of acetonitrile-water for gradient elution at 0.3 mL·min-1. The detection wavelength was 203 nm. Results:The calibration curves of typhaneoside,calycosin-7-O-β-D-glucopyranoside,isorhamnetin-3-O-neohesperidoside,ononin,notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1,and ginsenoside Rd were in good linearity over the ranges of 1.92-36.94 ng(r=0.999 8),1.90-36.63 ng(r=0.999 9),1.88-36.20 ng(r=0.999 6),0.99-19.09 ng(r=0.999 2),40.04-770.05 ng(r=0.999 8),107.78-2 072.68 ng(r=0.999 8),31.74-610.34 ng(r=0.999 1),81.33-1 564.08 ng(r=0.999 9),19.71-379.06 ng(r=0.999 9),respectively. The average recoveries(n=6) varied from 91%-105% with RSDs no more than 3.0%. The content ranges of the above mentioned 9 components in 3 batches of samples were 0.261-0.294,0.196-0.209,0.189-0.193,0.101-0.111,2.728-2.773,12.051-12.196,3.235-3.313,8.317-8.464,and 2.131-2.229 mg·g~(-1),respectively. Conclusion:This method can be used for quality control of Sanhuang Jingshiming pills.
Objective:To establish a UPLC method for the simultaneous determination of nine constituents in Sanhuang Jingshiming pills,including typhaneoside,calycosin-7-O-β-D-glucopyranoside,isorhamnetin-3-O-neohesperidoside,ononin,notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1,and ginsenoside Rd. Methods:The UPLC analysis was carried out by a 30 ℃ thermostatic Waters Acquity UPLC? BEH C18 column(2.1 mm×100 mm,1.7 μm) with a mobile phase composed of acetonitrile-water for gradient elution at 0.3 mL·min-1. The detection wavelength was 203 nm. Results:The calibration curves of typhaneoside,calycosin-7-O-β-D-glucopyranoside,isorhamnetin-3-O-neohesperidoside,ononin,notoginsenoside R1,ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1,and ginsenoside Rd were in good linearity over the ranges of 1.92-36.94 ng(r=0.999 8),1.90-36.63 ng(r=0.999 9),1.88-36.20 ng(r=0.999 6),0.99-19.09 ng(r=0.999 2),40.04-770.05 ng(r=0.999 8),107.78-2 072.68 ng(r=0.999 8),31.74-610.34 ng(r=0.999 1),81.33-1 564.08 ng(r=0.999 9),19.71-379.06 ng(r=0.999 9),respectively. The average recoveries(n=6) varied from 91%-105% with RSDs no more than 3.0%. The content ranges of the above mentioned 9 components in 3 batches of samples were 0.261-0.294,0.196-0.209,0.189-0.193,0.101-0.111,2.728-2.773,12.051-12.196,3.235-3.313,8.317-8.464,and 2.131-2.229 mg·g~(-1),respectively. Conclusion:This method can be used for quality control of Sanhuang Jingshiming pills.
引文
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[12]徐容.妇科千金片HPLC特征指纹图谱及多成分含量测定[J].中国实验方剂学杂志,2017,23(11):84XU R.Fingerprint and multi-component quantitative determination of Fuke Qianjin tablets by HPLC[J].Chin J ExpTradit Med Form,2017,23(11):84
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[14]杨秀青,石征蓉,谷江华,等.银菊解毒口服液指纹图谱结合多指标成分定量测定的质量控制方法研究[J].中草药,2017,48(13):2645YANG XQ,SHI ZR,GU JH,et al.Quality assessment of Yinju Jiedu oral liquid based on HPLC fingerprint and multi-components simultaneous determination[J].Chin Tradit Herb Drugs,2017,48(13):2645
[15]翟宏宇,王海洋,杨献玲,等.保心宁片HPLC特征图谱研究及8个指标性成分的含量测定[J].药物分析杂志,2017,37(9):1633ZHAI HY,WANG HY,YANG XL,et al.Study on HPLC specific chromatogram of Baoxinning tablets and simultaneous determination of its eight index components[J].Chin J Pharm Anal,2017,37(9):16332017 12 23
[2]焦增华,杨亚军,刘希望,等.蒲黄药理作用研究进展[J].中兽医医药杂志,2017,36(3):85JIAO ZH,YANG YJ,LIU XW,et al.Research advances in extraction and detection of ursolic acid and oleanolic acid[J].JTradit Chin Vet Med,2017,36(3):85
[3]胡立宏,房士明,刘虹,等.蒲黄的化学成分和药理活性研究进展[J].天津中医药大学学报,2016,35(2):136HU LH,FANG SM,LIU H,et al.Research progress in chemical ingredients and pharmacoactive of Puhuang[J].J Tianjin Univ TCM,2016,35(2):136
[4]祁晓霞,董宇,单晨啸,等.基于UFLC-Q-TOF/MS分析黄芪-丹参药对化学成分研究[J].南京中医药大学学报,2017,33(1):93QI XX,DONG Y,SHAN CX,et al.Analysis of the main components in herbal pair:Astragali Radix and Salviae Miltiorrhizae by UFLC-Q-TOF/MS[J].J Nanjing Univ Tradit Chin Med,2017,33(1):93
[5]石剑.黄芪中异黄酮成分的药代动力学特征及肝肠处置机制研究[D].广州:南方医科大学,2016SHI J.Pharmacokinetics and Enterohepatic Disposition of Isoflavonoids of Astragali Radix[D].Guangzhou:Southern Medical University,2016
[6]屠万倩,张留记,徐贞贞.HPLC法同时测定益心血脂康胶囊中3种成分[J].中成药,2017,39(2):316TU WQ,ZHANG LJ,XU ZZ.Simultaneous determination of three constituents in Yixin Xuezhikang capsules by HPLC[J].Chin Tradit Pat Med,2017,39(2):316
[7]张蔚,江曙,钱大玮,等.芒柄花苷与人体肠道细菌的相互作用研究[J].药学学报,2014,49(8):1162ZHANG W,JIANG S,QIAN DW,et al.The interaction between ononin and human intestinal bacteria[J].Acta Pharm Sin,2014,49(8):1162
[8]宋侠.三七皂苷药理作用研究进展[J].中国现代药物应用,2017,11(14):174SONG X.Recent advances in the research of pharmacological activities of Panax notoginseng saponins[J].Chin J Mod Drug Appl,2017,11(14):174
[9]泰瑞清,谈文状,杨恩,等.LC-MS分析三七根腐病的皂苷类成分变化[J].昆明理工大学学报(自然科学版),2015,40(6):85TAI RQ,TAN WZ,YANG E,et al.Variation of saponins in Panax notoginseng root rot diseases by LC-MS[J].J Kunming Univ Sci Technol(Nat Sci Ed),2015,40(6):85
[10]张华,刘俊萍,王菲菲,等.五味沙棘颗粒特征图谱及含量测定方法研究[J].药物分析杂志,2017,37(9):1627ZHANG H,LIU JP,WANG FF,et al.Study on characteristic fingerprint and quantitative analysis of Wuwei Shaji granules[J].Chin J Pharm Anal,2017,37(9):1627
[11]王艳伟,王青晓,王晓伟,等.HPLC波长切换法测定麦味地黄胶囊中5种有效成分的含量[J].药物分析杂志,2017,37(9):1601WANG YW,WANG QX,WANG XW,et al.Simultaneous determination of five constituents in Maiwei Dihuang capsules by HPLC with wavelength switching[J].Chin J Pharm Anal,2017,37(9):1601
[12]徐容.妇科千金片HPLC特征指纹图谱及多成分含量测定[J].中国实验方剂学杂志,2017,23(11):84XU R.Fingerprint and multi-component quantitative determination of Fuke Qianjin tablets by HPLC[J].Chin J ExpTradit Med Form,2017,23(11):84
[13]吕燕男,夏忠庭,李响,等.三黄睛视明丸UPLC指纹图谱[J].中成药,2018,40(4):880LüYN,XIA ZT,LI X,et al.UPLC fingerprints of Sanhuang Jingshiming pills[J].Chin Tradit Pat Med,2018,40(4):880
[14]杨秀青,石征蓉,谷江华,等.银菊解毒口服液指纹图谱结合多指标成分定量测定的质量控制方法研究[J].中草药,2017,48(13):2645YANG XQ,SHI ZR,GU JH,et al.Quality assessment of Yinju Jiedu oral liquid based on HPLC fingerprint and multi-components simultaneous determination[J].Chin Tradit Herb Drugs,2017,48(13):2645
[15]翟宏宇,王海洋,杨献玲,等.保心宁片HPLC特征图谱研究及8个指标性成分的含量测定[J].药物分析杂志,2017,37(9):1633ZHAI HY,WANG HY,YANG XL,et al.Study on HPLC specific chromatogram of Baoxinning tablets and simultaneous determination of its eight index components[J].Chin J Pharm Anal,2017,37(9):16332017 12 23