浙麦冬黄酮类成分指纹图谱及2种黄酮类化合物的含量测定
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摘要
目的:建立浙麦冬黄酮类成分的HPLC指纹图谱,并同时测定甲基麦冬二氢高异黄酮A和甲基麦冬二氢高异黄酮B的含量,为浙麦冬药材的质量控制提供依据。方法:采用Kromasil 100-5 C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.1%磷酸溶液(58∶42),流速1.0 m L·min-1,柱温30℃。结果:建立了浙麦冬黄酮类成分的HPLC指纹图谱,检出共有峰7个,各批次药材的相似度均>0.9;通过HPLC-MS分析和对照品比对,确定了1号峰和2号峰分别为甲基麦冬二氢高异黄酮A和甲基麦冬二氢高异黄酮B,并对其进行定量分析,结果浙麦冬中甲基麦冬二氢高异黄酮A的线性范围31.47~786.8 ng,平均回收率101.5%,甲基麦冬二氢高异黄酮B的线性范围53.05~1 326.25 ng,平均回收率103.0%。结论:HPLC指纹图谱方法与含量测定方法简便,结果准确,重复性好,可作为浙麦冬的质量控制方法。
Objective: To establish the HPLC fingerprints of flavonoids in Ophiopogonis Radix of Zhejiang and simultaneously determine the contents of methylophiopogonanone A and methylophiopogonanone B.Method: The chromatographic method was carried out on Kromasil 100-5 C18column( 4. 6 mm × 250 mm,5 μm)using acetonitrile-0. 1% phosphoric acid( 58∶ 42) as the mobile phase. The flow rate was 1. 0 m L·min- 1; and the column temperature was 30 ℃. Result: The HPLC fingerprints of Ophiopogonis Radix of Zhejiang were established and 7 common peaks were defined in the HPLC fingerprints. The similarity among different batches was above0. 9. By HPLC-MS analysis and comparison with standard reference substance, No. 1 peak was determined as methylophiopogonanone A and No. 2 peak was determined as methylophiopogonanone B. In the quantitative analysis of these two compounds,we found that the linear range was 31. 47-786. 8 ng for methylophiopogonanone A( R2= 1. 000 0) and 53. 05-1 326. 25 ng for methylophiopogonanone B( R2= 1. 000 0),and the average recovery rate( n = 6) was 101. 5% for methylophiopogonanone A and 103. 0% for methylophiopogonanone B. Conclusion:The HPLC fingerprint method and content determination method are simple,accurate with good reproducibility,and can be applied in the quality control of Ophiopogonis Radix of Zhejiang.
Objective: To establish the HPLC fingerprints of flavonoids in Ophiopogonis Radix of Zhejiang and simultaneously determine the contents of methylophiopogonanone A and methylophiopogonanone B.Method: The chromatographic method was carried out on Kromasil 100-5 C18column( 4. 6 mm × 250 mm,5 μm)using acetonitrile-0. 1% phosphoric acid( 58∶ 42) as the mobile phase. The flow rate was 1. 0 m L·min- 1; and the column temperature was 30 ℃. Result: The HPLC fingerprints of Ophiopogonis Radix of Zhejiang were established and 7 common peaks were defined in the HPLC fingerprints. The similarity among different batches was above0. 9. By HPLC-MS analysis and comparison with standard reference substance, No. 1 peak was determined as methylophiopogonanone A and No. 2 peak was determined as methylophiopogonanone B. In the quantitative analysis of these two compounds,we found that the linear range was 31. 47-786. 8 ng for methylophiopogonanone A( R2= 1. 000 0) and 53. 05-1 326. 25 ng for methylophiopogonanone B( R2= 1. 000 0),and the average recovery rate( n = 6) was 101. 5% for methylophiopogonanone A and 103. 0% for methylophiopogonanone B. Conclusion:The HPLC fingerprint method and content determination method are simple,accurate with good reproducibility,and can be applied in the quality control of Ophiopogonis Radix of Zhejiang.
引文
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[7]白晶.麦冬甾体皂苷和高异黄酮类成分的研究进展[J].北京联合大学学报,2014,28(2):9-12.
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[2]林以宁,志田保夫,袁博,等.不同产地麦冬的指纹图谱比较研究[J].中国药科大学学报,2005,36(6):538-542.
[3]陈有根,邬国庆,戴俊东,等.麦冬指纹图谱研究[J].中国中医药信息杂志,2008,15(4):56-58.
[4]车晓彦,伍丕娥,周娟,等.麦冬药材TLC及HPLC特征图谱研究[J].药物分析杂志,2012,32(12):2262-2266.
[5]贾诚,叶正良,姜秀晶,等.川麦冬药材中黄酮类成分HPLC指纹图谱的研究[J].辽宁中医杂志,2011,38(6):1182-1184.
[6]王进,刘汉清,刘霖,等.HPLC定量指纹图谱法评价川麦冬质量研究[J].中药材,2013,36(5):721-725.
[7]白晶.麦冬甾体皂苷和高异黄酮类成分的研究进展[J].北京联合大学学报,2014,28(2):9-12.
[8]周一峰,戚进,朱丹妮,等.麦冬须根高异黄酮类成分及其清除氧自由基作用[J].中国天然药物,2008,6(3):201-204.