亚麻籽环肽HPLC分析和氧化还原产物研究
HPLC analysis of flaxseed cyclolinopeptides and their oxidation and reduction products
  
DOI:
中文关键词:  亚麻籽环肽  氧化还原  分离纯化  HPLC
英文关键词:flaxseed cyclolinopeptide  oxidation and reduction  separation and purification  HPLC
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Author NameAffiliation
ZUO Yang  
LU Xuerong  
TENG Yinglai,etc  
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中文摘要:
      对从天然亚麻籽中提取的粗环肽的组分和氧化还原性质进行探讨。采用HPLC测定亚麻籽粗环肽中环肽C(CLC)、环肽E(CLE)、环肽D(CLD)、环肽A(CLA)的含量,并通过还原的方法减少粗环肽中的环肽种类,以制备环肽单体。结果表明,环肽样品峰分离度良好,线性范围 10~150 μg/mL(环肽A的为10~100 μg/mL),相关系数0.999 0~0.999 7。所测4种环肽的含量分别为CLC 8.10%,CLE 7.66%,CLD 0.58%,CLA 35.18%。粗环肽经过氧化或还原反应之后,其种类均发生改变。经HPLC定性分析,氧化后剩余6种环肽,还原后的环肽仅剩下4种,通过与已知峰对比,得知4种环肽分别为环肽B、环肽L、环肽A和环肽M,在C18分析柱上分离良好,以此为理论依据,采用Microsorb 100-5 C18制备柱(240 mm×21.4 mm),柱温30℃,流速5 mL/min,70%乙腈溶液等度洗脱,在50 min内可有效分离制备环肽单体。
英文摘要:
      The composition and oxidation and reduction properties of crude cyclolinopeptides extracted from natural flaxseed were studied. HPLC was employed to detect the contents of cyclolinopeptide C(CLC), cyclolinopeptide E(CLE), cyclolinopeptide D(CLD) and cyclolinopeptide A(CLA) in crude flaxseed cyclolinopeptides. Reduction was used to aid the separation of monomer as it could reduce the types of cyclolinopeptide in the crude cyclolinopeptides effectively. The results indicated that the cyclolinopeptides were separated well, and the linear range and correlation coefficient were 10-150 μg/mL(10-100 μg/mL for CLA) and 0999 0-0999 7, respectively. The contents of CLC, CLE, CLD and CLA in the crude cyclolinopeptides were 8.10%, 7.66%, 0.58% and 35.18% respectively. The cyclolinopeptide type in crude cyclolinopeptides could be transformed by oxidation or reduction reaction. According to the results of qualitative HPLC analysis, 6 cyclolinopeptides were left after oxidation, while only 4 cyclolinopeptides were left after reduction and were respectively determined as CLB, CLL, CLA and CLM by comparing with the standard cyclolinopeptides. Besides, they were separated well by C18 column, based on this, singular cyclolinopeptide was separated effectively in 50 min by preparative HPLC using Microsorb 100-5 C18 column (240 mm × 21.4 mm) under the conditions of column temperature 30℃, flow rate 5 mL/min and an isocratic elution of 70% acetonitrile solution.
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