HPLC波长切换法同时测定益安宁丸中7种活性成分
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摘要
目的建立HPLC波长切换法同时测定益安宁丸中7种活性成分的方法。方法采用HPLC法,同时测定益安宁丸中三七皂苷R_1、五味子醇甲、丹酚酸B、五味子酯甲、人参皂苷Rg_1、人参皂苷Rb_1、丹参酮Ⅱ_A的含量,采用Shim-pack GIST-C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱:0～5 min,5%乙腈;5～12 min,5%～12%乙腈;12～17 min,12%～20%乙腈;17～30 min,20%乙腈;30～36 min,20%～50%乙腈;36～45 min,50%～80%乙腈;45～70 min,80%乙腈;检测波长203 nm(三七皂苷R_1、人参皂苷Rg_1、人参皂苷Rb_1)、220 nm(五味子酯甲)、250nm(五味子醇甲)、268nm(丹酚酸B)和270nm(丹参酮Ⅱ_A),体积流量1.0 mL/min,柱温35℃,进样量10μL。结果三七皂苷R_1、五味子醇甲、丹酚酸B、五味子酯甲、人参皂苷Rg_1、人参皂苷Rb_1、丹参酮Ⅱ_A检测质量浓度的线性范围分别为0.015～0.150、0.077～0.766、0.006～0.062、0.009～0.092、0.050～0.503、0.067～0.670、0.011～0.108 mg/mL;平均加样回收率分别为99.5%、99.8%、99.2%、98.9%、96.9%、98.8%、97.1%。结论该方法简单、有效、结果准确,可用于益安宁丸中上述7种活性成分的同时测定。
Objective To establish an HPLC method for the simultaneous content determination of seven constituents in Compound Yi'anning Pills(CYP). Methods The determination was performed on Shim-pack GIST C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid(gradient elution: 0—5 min, 5% acetonitrile; 5—12 min, 5%—12% acetonitrile; 12—17 min, 12%—20% acetonitrile; 17—30 min, 20% acetonitrile; 30—36 min, 20%—50% acetonitrile; 36—45 min, 50%—80% acetonitrile; 45—70 min, 80% acetonitrile) at the flow rate of 1.0 mL/min. The detection wavelength was set at 203 nm for notoginsenoside R_1, ginsenoside Rg_1, and ginsenoside Rb_1, 220 nm for schisantherrin A, 250 nm for schisandrin, 268 nm for salvianolic acid B, and 270 nm for tanshinone Ⅱ_A. The column temperature was set at 35 ℃ and the injection volume was 10 μL. Results The linear range of detection concentration was 0.015—0.150 mg/mL for notoginsenoside R_1, 0.077—0.766 mg/mL for schisandrin, 0.006—0.062 mg/m L for salvianolic acid B, 0.009—0.092 mg/mL for buddleodide, 0.050—0.503 mg/m L for ginsenoside Rg_1, 0.067—0.670 mg/m L for ginsenoside Rb_1, and 0.011—0.108 mg/mL for tanshinone Ⅱ_A. Average recoveries respectively were 99.5%, 99.8%, 99.2%, 98.9%, 96.9%, 98.8%, and 97.1%. Conclusion The method is simple, effective, and accurate, which can be used for simultaneous determination of seven active constituents in CYP.
Objective To establish an HPLC method for the simultaneous content determination of seven constituents in Compound Yi'anning Pills(CYP). Methods The determination was performed on Shim-pack GIST C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid(gradient elution: 0—5 min, 5% acetonitrile; 5—12 min, 5%—12% acetonitrile; 12—17 min, 12%—20% acetonitrile; 17—30 min, 20% acetonitrile; 30—36 min, 20%—50% acetonitrile; 36—45 min, 50%—80% acetonitrile; 45—70 min, 80% acetonitrile) at the flow rate of 1.0 mL/min. The detection wavelength was set at 203 nm for notoginsenoside R_1, ginsenoside Rg_1, and ginsenoside Rb_1, 220 nm for schisantherrin A, 250 nm for schisandrin, 268 nm for salvianolic acid B, and 270 nm for tanshinone Ⅱ_A. The column temperature was set at 35 ℃ and the injection volume was 10 μL. Results The linear range of detection concentration was 0.015—0.150 mg/mL for notoginsenoside R_1, 0.077—0.766 mg/mL for schisandrin, 0.006—0.062 mg/m L for salvianolic acid B, 0.009—0.092 mg/mL for buddleodide, 0.050—0.503 mg/m L for ginsenoside Rg_1, 0.067—0.670 mg/m L for ginsenoside Rb_1, and 0.011—0.108 mg/mL for tanshinone Ⅱ_A. Average recoveries respectively were 99.5%, 99.8%, 99.2%, 98.9%, 96.9%, 98.8%, and 97.1%. Conclusion The method is simple, effective, and accurate, which can be used for simultaneous determination of seven active constituents in CYP.
引文
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[16]胡玉飘,崔秀明,张泽君,等.失效模式分析和星点设计-效应面法优化熟三七皂苷类成分纯化工艺[J].中草药,2018,49(13):3009-3016.
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[19]刘慧颖,王承潇,杨野,等.微波辅助降解三七茎叶总皂苷生成人参皂苷Rg5的工艺研究[J].中草药,2018,49(14):3245-3251.
[20]代晓光,苏长兰.丹参化学成分及药理研究进展[J].中医药信息,2018,35(4):126-129.
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[23]代琪,罗霄,叶俏波.HPLC测定益安宁丸中西洋参和三七的有效成分[J].重庆中草药研究,2017,36(2):20-26.
[2]张群豪,李海霞.益安宁治疗冠心病心绞痛60例临床观察[J].疑难病杂志,2006,5(6):411-414.
[3]蔡少杭,吴怡萍.益安宁治疗慢性疲劳综合征30例临床观察[J].实用中医内科杂志,2014,28(1):42-44.
[4]张岚,王平,张涛.益安宁丸联合二丁酰环磷腺苷钙对慢性心力衰竭患者心肺功能及血清MMP-9、BNP水平的影响[J].中药药理与临床,2017,33(6):146-148.
[5]林红强,李平亚,刘金平.野生西洋参鉴别、化学成分及药理作用研究进展[J].天然产物研究与开发,2017,29(12):2157-2162.
[6]刘鹏,王士伟,夏广萍.西洋参花蕾中人参皂苷Re、拟人参皂苷F11、人参皂苷Rb3、人参皂苷Rd的含量测定[J].中草药,2018,49(17):4144-4147.
[7]白雪,黄鑫,刘淑莹.不同来源西洋参药材及产品皂苷成分评价研究[J].药物评价研究,2015,38(6):652-655.
[8]荆然,李慧峰,程艳刚,等.五味子不同炮制品对小鼠慢性不可预知性应激抑郁的改善作用[J].现代药物与临床,2016,31(11):1698-1702.
[9]王馨雅,高慧,王晓婷,等.五味子不同炮制品对大鼠肾阳虚的改善作用研究[J].现代药物与临床,2018,33(1):10-14.
[10]张琨琨.五味子多糖免疫调节及抗氧化功能研究[J].职业卫生与病伤,2016,31(1):54-57.
[11]苏联麟,李平,程雪,等.基于UPLC-Q/TOF-MS的醋制五味子对酒精性肝损伤大鼠胆汁代谢物的影响研究[J].中草药,2017,48(1):114-120.
[12]任海风,王世华.五味子药理作用研究进展[J].中国医院用药评价与分析,2018,18(8):1151-1152.
[13]杨擎,曲晓波,李辉,等.五味子化学成分与药理作用研究进展[J].吉林中医药,2015,35(6):626-628.
[14]周永峰,李瑞煜,张定堃,等.基于UPLC-Q-TOF/MS的五味子不同部位化学成分研究[J].中草药,2017,48(6):1087-1092.
[15]杨娟,袁一怔,尉广飞,等.三七植物化学成分及药理作用研究进展[J].世界科学技术-中医药现代化,2017,19(10):1641-1647.
[16]胡玉飘,崔秀明,张泽君,等.失效模式分析和星点设计-效应面法优化熟三七皂苷类成分纯化工艺[J].中草药,2018,49(13):3009-3016.
[17]周晨,刘辉.三七功用与化学成分[J].实用中医内科杂志,2018,32(8):4-7.
[18]Yang J,Dong L L,Wei G F,et al.Identification and quality analysis of Panax notoginseng and Panax vietnamensis var.fuscidicus through integrated DNAbarcoding and HPLC[J].Chin Herb Med,2018,10(2):176-182.
[19]刘慧颖,王承潇,杨野,等.微波辅助降解三七茎叶总皂苷生成人参皂苷Rg5的工艺研究[J].中草药,2018,49(14):3245-3251.
[20]代晓光,苏长兰.丹参化学成分及药理研究进展[J].中医药信息,2018,35(4):126-129.
[21]罗志毅,包国荣.HPLC法测定益安宁中人参皂苷Rb1的含量[J].海峡药学,2006,18(2):48-50.
[22]王柯,季申.益安宁丸中人参皂苷Rg1、Re和Rb1的HPLC测定[J].中国医药工业杂志,2004,35(10):33-34.
[23]代琪,罗霄,叶俏波.HPLC测定益安宁丸中西洋参和三七的有效成分[J].重庆中草药研究,2017,36(2):20-26.