止动颗粒UPLC指纹图谱建立及3种成分测定
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摘要
目的建立止动颗粒UPLC指纹图谱,并测定其中3种成分的含量。方法以黄芩苷为参照峰,建立11批样品的UPLC指纹图谱,采用Acquity HSS T3色谱柱(150 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,体积流量0.3mL/min,柱温40℃,检测波长254nm,测定黄芩苷、栀子苷和芍药苷的含量。结果建立了UPLC指纹图谱,鉴定了没食子酸、车叶草苷、去乙酰车叶草苷酸甲酯、绿原酸、京尼平1-β-D-龙胆双糖苷、栀子苷、芍药苷、白杨素-6-C-β-D-葡萄糖-8-C-α-L-阿拉伯糖苷、白杨素-6-C-α-L-阿拉伯吡喃糖-8-C-β-D-葡萄糖苷、白杨素-6-C-α-L-阿拉伯吡喃糖-8-C-β-D-葡萄糖苷异构体、黄芩苷、黄芩苷异构体、千层纸素A-7-O-葡萄糖醛酸苷、汉黄芩苷、汉黄芩素、五味子醇甲16个成分,11批制剂相似度达到0.98以上。黄芩苷、栀子苷、芍药苷分别在12.15～388.80μg/mL、6.52～209.00μg/mL、8.38～268.00μg/mL线性关系良好,平均加样回收率(RSD)分别为100.98%(3.04%)、100.49%(0.60%)、100.55%(2.73%)。11批制剂中黄芩苷为7.46～12.40 mg/g,栀子苷为7.01～13.27 mg/g,芍药苷为7.68～12.76 mg/g。结论该方法准确简单,稳定可靠,可用于止动颗粒质量控制。
Objective To establish the UPLC fingerprints of Zhidong Granules(ZG) and determine the content of three constituents.Methods With baicalin as a reference peak,the UPLC fingerprints of 11 batches of samples were established.The analysis of ZG was performed on a 40 ℃ thermostatic Acquity HSS T3 column(150 mm × 2.1 mm,1.8 μm),with the mobile phase comprising of acetonitrile-0.1% formic acid flowing at 0.3 mL/min in a gradient elution manner,and the detection wavelength was set at 254 nm.Results The UPLC fingerprint was established and 16 components were identified(gallic acid,asperuloside,methyl deacetylcyrrhizin,chlorogenic acid,genipin 1-gentiobioside,geniposide,paeoniflorin,chrysin-6-C-β-D-glucopyranosyl-8-C-α-Larabinopyranoside,chrysin-6-C-α-L-arabopylanose-8-C-β-D-glucoside or isomer,baicalin,baicalin isomer,oroxylin A-7-Oglucuronide,wogonoside,wogonin,and schizandrin).The similarity of 11 batches of preparations were at least 0.98.Baicalin,paeoniflorin,and geniposide showed good linear relationships within the ranges of 12.15—388.80 μg/mL,6.52—209.00 μg/mL,and 8.38—268.00 μg/mL,whose average recoveries(RSD) were 100.98%(3.04%),100.49%(0.60%),and 100.55%(2.73%),respectively.The content of baicalin in the 11 batches of preparations was between 7.46 and 12.40 mg/g,the content of geniposide was between 7.01 and 13.27 mg/g,and the content of paeoniflorin was between 7.68 and 12.76 mg/g.Conclusion The method is accurate,simple,stable,and reliable,and can be used for quality control of ZG.
Objective To establish the UPLC fingerprints of Zhidong Granules(ZG) and determine the content of three constituents.Methods With baicalin as a reference peak,the UPLC fingerprints of 11 batches of samples were established.The analysis of ZG was performed on a 40 ℃ thermostatic Acquity HSS T3 column(150 mm × 2.1 mm,1.8 μm),with the mobile phase comprising of acetonitrile-0.1% formic acid flowing at 0.3 mL/min in a gradient elution manner,and the detection wavelength was set at 254 nm.Results The UPLC fingerprint was established and 16 components were identified(gallic acid,asperuloside,methyl deacetylcyrrhizin,chlorogenic acid,genipin 1-gentiobioside,geniposide,paeoniflorin,chrysin-6-C-β-D-glucopyranosyl-8-C-α-Larabinopyranoside,chrysin-6-C-α-L-arabopylanose-8-C-β-D-glucoside or isomer,baicalin,baicalin isomer,oroxylin A-7-Oglucuronide,wogonoside,wogonin,and schizandrin).The similarity of 11 batches of preparations were at least 0.98.Baicalin,paeoniflorin,and geniposide showed good linear relationships within the ranges of 12.15—388.80 μg/mL,6.52—209.00 μg/mL,and 8.38—268.00 μg/mL,whose average recoveries(RSD) were 100.98%(3.04%),100.49%(0.60%),and 100.55%(2.73%),respectively.The content of baicalin in the 11 batches of preparations was between 7.46 and 12.40 mg/g,the content of geniposide was between 7.01 and 13.27 mg/g,and the content of paeoniflorin was between 7.68 and 12.76 mg/g.Conclusion The method is accurate,simple,stable,and reliable,and can be used for quality control of ZG.
引文
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[18]刘大伟,闫广利,方圆,等.UPLC-ESI-TOF/MS应用于黄芩化学成分的快速分析[J].中医药信息,2012,29(4):20-24.
[19]郑勇凤,王佳婧,傅超美,等.黄芩的化学成分与药理作用研究进展[J].中成药,2016,38(1):141-147.
[20]李伟,刘亚丽,宋永贵,等.UPLC-Q-TOF-MSE结合OPLS-DA模式快速鉴定南、北五味子化学成分与识别差异标志物[J].中草药,2015,46(15):2212-2218.
[2]杨书美.滇龙胆指纹图谱的研究[D].哈尔滨:哈尔滨商业大学,2015.
[3]夏菁,谢媛媛,张宗璇,等.骨通贴膏指纹图谱及化学成分研究[J].中成药,2014,36(3):571-576.
[4]史静超,张俊杰,高晓霞,等.龟龄集胶囊无机元素指纹图谱的建立及主成分分析[J].中草药,2018,49(15):3619-3624.
[5]Xie R F,Zhao Q H,Li Z C,et al.Comparison on HPLCfingerprints between Fraxini Cortex and its eye drop[J].Chin Herb Med,2013,5(4):301-306.
[6]周桂荣,李响,赵桂铃,等.橘叶UPLC指纹图谱和化学模式识别研究[J].药物评价研究,2018,41(12):2237-2241.
[7]康建,周霖,孙志,等.基于UPLC指纹图谱结合化学模式识别的冠心丹参胶囊质量控制研究[J].中草药,2018,49(17):4051-4057.
[8]秦建平,吴建雄,郎悦,等.痛宁凝胶的HPLC-MS指纹图谱研究[J].现代药物与临床,2016,31(4):427-430.
[9]高青,刘颖,宋彬彬,等.超高效液相色谱与高效液相色谱方法转换及验证[J].药物分析杂志,2016,36(7):1279-1286.
[10]齐炼文,杨华,李会军,等.中药有效成分群发现与质量评价研究[A]//第三届中国天然药物研究与发展论坛论文集[C].南京:中国药学会,2013.
[11]陈晓虎,苏晶,王慧,等.UPLC法同时测定栀子金花丸中11种成分[J].中草药,2014,45(7):955-959.
[12]孙东东,徐晓芳,崔九成,等.白芍水提部位化学成分的HPLC-ESI-Q-TOF-MS分析[J].中国中药杂志,2013,38(11):1760-1765.
[13]Wang L,Liu S,Zhang X,et al.A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry[J].J Chromatogr A,2016,1452(6):47-57.
[14]娄素卉.中药材栀子的化学物质基础研究[D].上海:华东理工大学,2012.
[15]王晓燕,张丽,王添琦,等.栀子化学成分的UHPLC-Q-TOFMS分析[J].中药材,2013,36(3):407-410.
[16]严欢,左月明,袁恩,等.基于UHPLC-Q-TOF-MS技术分析栀子花中的化学成分[J].中药材,2018,41(6):1359-1364.
[17]邵怡,杨玉佩,陈林,等.HPLC-Q-TOF-MS/MS分析防风芍药汤水煎液的化学成分[J].中国实验方剂学杂志,2018,24(8):54-59.
[18]刘大伟,闫广利,方圆,等.UPLC-ESI-TOF/MS应用于黄芩化学成分的快速分析[J].中医药信息,2012,29(4):20-24.
[19]郑勇凤,王佳婧,傅超美,等.黄芩的化学成分与药理作用研究进展[J].中成药,2016,38(1):141-147.
[20]李伟,刘亚丽,宋永贵,等.UPLC-Q-TOF-MSE结合OPLS-DA模式快速鉴定南、北五味子化学成分与识别差异标志物[J].中草药,2015,46(15):2212-2218.