盐黄柏一测多评法色谱评价系统的建立
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摘要
目的建立盐黄柏一测多评法色谱评价系统,优选盐黄柏色谱条件,对盐黄柏进行质量控制研究。方法采用HLPC法测定盐黄柏中盐酸小檗碱、木兰花碱、盐酸小檗红碱、黄柏碱、巴马汀、药根碱6种生物碱含量,以峰宽、对称因子、分离度综合评分为评价指标,考察流动相系统组成、流动相p H值、色谱柱以及柱温,优选盐黄柏一测多评法色谱条件,并通过7个不同厂家,10批盐黄柏药材进行验证。结果确定盐黄柏多成分含量测定方法条件为色谱柱:Inertsil ODS-3 5μm4.6×250mm流动相:乙腈:0.1%磷酸(15:85);柱温:30℃;流速:1ml·min~(-1);进样量:5μL;检测波长:265nm。结论该色谱条件下,各峰对称性良好、峰宽较窄、分离度好,用于盐黄柏多成分含量测定稳定、可行。全面地反映盐黄柏药材中化学成分的信息,可为盐黄柏药材的研究以及质量标准制定提供科学依据。
Objective To establish chromatographic evaluation system for determination of multi-component constituents for Cortex Phellodendri at the first time. The quality of Cortex Phellodendri were conducted on quantitative studies. Methods Investigate the effects of mobile phase composition,p H value,column and column temperature on the HLPC method for the determination of six alkaloids in Cortex Phellodendri,including berberine hydrochloride, magnoflorine, berberubine, phellodendrine, palmatine, jatrorrhizine. Verified by determining 10 batches of salt Phellodendron in different factories. Results The best separation conduction was IInertsil ODS-3 5μm 4. 6* 250 mm( with mobile phase composed of acetonitrile -0. 1% phosphoric acid solution for gradient elution at the flow rate of 1. 0 ml·min~(-1),the column temperature at 30℃,the injection volume was 5 μL,the detection wavelength at 265 nm. Conclusion For the first time,a method for the determination of the constituents in Cortex Phellodendri and its HLPC fingerprinting were established. The qualitative and quantitative analysis of the Cortex Phellodendri can reflect the information of chemical constituents in the medicinal materials,and provide the scientific basis for the study of the medicinal materials and the establishment of the quality standard.
Objective To establish chromatographic evaluation system for determination of multi-component constituents for Cortex Phellodendri at the first time. The quality of Cortex Phellodendri were conducted on quantitative studies. Methods Investigate the effects of mobile phase composition,p H value,column and column temperature on the HLPC method for the determination of six alkaloids in Cortex Phellodendri,including berberine hydrochloride, magnoflorine, berberubine, phellodendrine, palmatine, jatrorrhizine. Verified by determining 10 batches of salt Phellodendron in different factories. Results The best separation conduction was IInertsil ODS-3 5μm 4. 6* 250 mm( with mobile phase composed of acetonitrile -0. 1% phosphoric acid solution for gradient elution at the flow rate of 1. 0 ml·min~(-1),the column temperature at 30℃,the injection volume was 5 μL,the detection wavelength at 265 nm. Conclusion For the first time,a method for the determination of the constituents in Cortex Phellodendri and its HLPC fingerprinting were established. The qualitative and quantitative analysis of the Cortex Phellodendri can reflect the information of chemical constituents in the medicinal materials,and provide the scientific basis for the study of the medicinal materials and the establishment of the quality standard.
引文
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[12]林芳,王云红,万丽,杨荣平.一测多评法结合指纹图谱对杜仲质量控制的研究[J].中国实验方剂学杂志,2012,18(13):78.
[2]王萌,吉腾飞,杨建波,等.川黄柏化学成分研究[J].中药材,2009,32(2):208.
[3]董凯旋,董立莎.黄柏饮片炮制规范化及质量控制的研究进展[J].贵阳中医学院学报,2011,33(2):78.
[4]唐永红,麻春恒,潘忠记.炮制盐黄柏新工艺参数优选的研究[J].广西医学,2006,47(9):1426.
[5]吴珊珊,胡昌江,吕非非,等.一测多评法测定黄柏中5种生物碱[J].中成药,2014,36(1):130.
[6]祁东利,贾天柱,廉莲.黄柏炮制后化学成分转化研究[J].中成药,2010,32(3):443.
[7]孔晶晶,朱晶晶,王智民,张启伟,高慧敏,闫利华.一测多评法测定连翘中多种不同类型成分的含量[J].中国药学杂志,2010,45(17):1301.
[8]李倩,刘伟,罗祖良,等.一测多评法测定丹参中丹参酮Ⅱ_A、隐丹参酮、丹参酮Ⅰ、二氢丹参酮Ⅰ的含量[J].中国中药杂志,2012,37(6):824.
[9]陈建维,刘圆,刘晟楠,等.一测多评法测定枳实中4种黄酮类成分[J].中草药,2015,46(09):1374.
[10]夏成凯,郭伟娜,王甫成,等.一测多评法测定紫菀中5种黄酮类成分含量[J/OL].中药材,2015,38(01):112.
[11]冯伟红,杨菲,王智民,等.一测多评法与外标法测定双黄连制剂中黄酮类成分含量的比较分析[J].中国药学杂志,2012,47(20):1665.
[12]林芳,王云红,万丽,杨荣平.一测多评法结合指纹图谱对杜仲质量控制的研究[J].中国实验方剂学杂志,2012,18(13):78.