目的建立超高效液相色谱-四极杆飞行时间质谱联用技术(ultra performance liquid chromatography quadrupole time of flight mass spectrometry,UPLC-Q-TOF-MS/MS)结合多元统计分析技术的分析方法,比较不同品种牛膝的化学成分差异。方...目的建立超高效液相色谱-四极杆飞行时间质谱联用技术(ultra performance liquid chromatography quadrupole time of flight mass spectrometry,UPLC-Q-TOF-MS/MS)结合多元统计分析技术的分析方法,比较不同品种牛膝的化学成分差异。方法基于UPLC-Q-TOF-MS/MS技术对怀牛膝Achyranthes bidentata、川牛膝Cyathula officinalis、红牛膝Cyathula capitata和土牛膝Achyranthes aspera的化学成分进行分析与鉴别,并运用多元统计分析筛选不同品种牛膝的差异性成分。结果共初步指认出230种化学成分,其中皂苷类81种、生物碱类26种、甾酮类12种、有机酸类75种、木脂素类19种和黄酮类17种。根据变量重要性投影(variable importance in projection,VIP)值>1,t检验(P<0.05)从4种牛膝中共筛选出25个化学标志物。其中,竹节参皂苷、牛膝皂苷在怀牛膝中占比居多;竹节参皂苷IVa在红牛膝中的占比最高;甾醇、黄酮醇、有机酸和糖苷类成分在川牛膝中的占比最高;齐墩果烷型皂苷和酪胺类生物碱类成分则在安徽土牛膝中占比最多。结论该方法快速、全面地对牛膝植物资源的成分进行系统分析,为牛膝的品种分类鉴别和资源开发利用提供了基础。展开更多
[Objectives] To determine the content of oleanolic acid in 10 batches of Achyranthes aspera L. from different production areas,and to establish a high performance liquid chromatography( HPLC) method for the determinat...[Objectives] To determine the content of oleanolic acid in 10 batches of Achyranthes aspera L. from different production areas,and to establish a high performance liquid chromatography( HPLC) method for the determination of oleanolic acid in A. aspera. [Methods]Agilent C18 liquid chromatography column( 250 mm × 4. 6 mm,5 μm) was used for gradient elution with acetonitrile∶ water = 61∶ 39 as the mobile phase. The flow rate was 1 mL/min,the detection wavelength was 210 nm,and the column temperature was 35℃. [Results] The oleanolic acid injection volume showed a good linear relationship with the peak area in the range of 0. 382-7. 640 μg. The linear equation of oleanolic acid was: A = 530. 76 C,R = 1. 000 0; the range of sample recovery rate was 96. 03%-102. 73%,and the RSD value was 2. 16%( n =9). The content of the oleanolic acid was the highest in A. aspera produced in Guilin City of Guangxi( 0. 92%),and the lowest oleanolic acid content was in sample of Sitang in Nanning City of Guangxi( 0. 27%). It is recommended that the oleanolic acid content of A. aspera should not be lower than 0. 20%. [Conclusions]The HPLC method is accurate,reliable,easy to operate,and has good resolution. It is suitable for the determination of the content of oleic acid in A. aspera. It can provide reference for the quality control and standard drafting of A. aspera.展开更多
文摘目的建立超高效液相色谱-四极杆飞行时间质谱联用技术(ultra performance liquid chromatography quadrupole time of flight mass spectrometry,UPLC-Q-TOF-MS/MS)结合多元统计分析技术的分析方法,比较不同品种牛膝的化学成分差异。方法基于UPLC-Q-TOF-MS/MS技术对怀牛膝Achyranthes bidentata、川牛膝Cyathula officinalis、红牛膝Cyathula capitata和土牛膝Achyranthes aspera的化学成分进行分析与鉴别,并运用多元统计分析筛选不同品种牛膝的差异性成分。结果共初步指认出230种化学成分,其中皂苷类81种、生物碱类26种、甾酮类12种、有机酸类75种、木脂素类19种和黄酮类17种。根据变量重要性投影(variable importance in projection,VIP)值>1,t检验(P<0.05)从4种牛膝中共筛选出25个化学标志物。其中,竹节参皂苷、牛膝皂苷在怀牛膝中占比居多;竹节参皂苷IVa在红牛膝中的占比最高;甾醇、黄酮醇、有机酸和糖苷类成分在川牛膝中的占比最高;齐墩果烷型皂苷和酪胺类生物碱类成分则在安徽土牛膝中占比最多。结论该方法快速、全面地对牛膝植物资源的成分进行系统分析,为牛膝的品种分类鉴别和资源开发利用提供了基础。
基金Supported by Special Project of Traditional Chinese Medicine Technology for Health Department of Guangxi Zhuang Autonomous Region(GZBZ14-09)China-ASEAN Traditional Medicine Development Research Center
文摘[Objectives] To determine the content of oleanolic acid in 10 batches of Achyranthes aspera L. from different production areas,and to establish a high performance liquid chromatography( HPLC) method for the determination of oleanolic acid in A. aspera. [Methods]Agilent C18 liquid chromatography column( 250 mm × 4. 6 mm,5 μm) was used for gradient elution with acetonitrile∶ water = 61∶ 39 as the mobile phase. The flow rate was 1 mL/min,the detection wavelength was 210 nm,and the column temperature was 35℃. [Results] The oleanolic acid injection volume showed a good linear relationship with the peak area in the range of 0. 382-7. 640 μg. The linear equation of oleanolic acid was: A = 530. 76 C,R = 1. 000 0; the range of sample recovery rate was 96. 03%-102. 73%,and the RSD value was 2. 16%( n =9). The content of the oleanolic acid was the highest in A. aspera produced in Guilin City of Guangxi( 0. 92%),and the lowest oleanolic acid content was in sample of Sitang in Nanning City of Guangxi( 0. 27%). It is recommended that the oleanolic acid content of A. aspera should not be lower than 0. 20%. [Conclusions]The HPLC method is accurate,reliable,easy to operate,and has good resolution. It is suitable for the determination of the content of oleic acid in A. aspera. It can provide reference for the quality control and standard drafting of A. aspera.
