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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10~150μg/m L(环肽A的为10~100μg/m L),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 m L/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。
The constituents and redox properties of the crude cyclic peptides extracted from natural flaxseed were investigated. The contents of cyclic peptide C (CLC), cyclopeptide E (CLE), cyclic peptide D (CLD) and cyclic peptide A (CLA) in the flaxseed crude peptide were determined by HPLC and the reduction of ring Peptide species to prepare cyclic peptide monomers. The results showed that the peak separation of cyclopeptide was good with a linear range of 10-150 μg / mL (cyclic peptide A: 10-100 μg / mL) with a correlation coefficient of 0.999 0-0.9997. The content of the four cyclic peptides measured were CLC 8.10%, CLE 7.66%, CLD 0.58%, CLA 35.18%. The crude cyclopeptide after oxidation or reduction reaction, its species have changed. According to the qualitative analysis of HPLC, the remaining six kinds of cyclic peptides remained after oxidation, and only four remaining cyclic peptides were recovered. By comparison with the known peaks, the four kinds of cyclic peptides were known as cyclic peptide B, cyclic peptide L, cyclic peptide A And Cyclic Peptide M were separated on a C18 column. Microsorb 100-5 C18 was used to prepare a column (240 mm × 21.4 mm) with a column temperature of 30 ℃, a flow rate of 5 mL / min, 70% acetonitrile Solution isocratic elution, within 50 min effective separation and preparation of cyclic peptide monomer.