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| HPLC测定亚麻籽油苦味肽的纯化富集前处理研究 |
| Pretreatment of purification and enrichment for determination of bitter peptides in flaxseed oil by HPLC |
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| DOI： |
| 中文关键词: 亚麻籽油 苦味肽 前处理 纯化富集 固相萃取法 |
| 英文关键词:flaxseed oil bitter peptides pretreatment purification and enrichment solid phase extraction method |
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| 中文摘要: |
| 比较了高效液相色谱（HPLC）定量测定亚麻籽油苦味肽(CLE)的溶剂萃取法和固相萃取法（SPE）纯化富集前处理效果，并对不同规格SPE硅胶小柱填料的前处理效果作了对比。结果表明，通过溶剂萃取法和固相萃取法前处理的亚麻籽油样品，进行HPLC定量测定时，CLE均可以在液相色谱中得到良好的分离，前处理方法并不影响CLE的出峰时间及峰形。但与溶剂萃取法相比，SPE所提取的环肽样品中甘油三酯及其他杂质显著减少，这有利于保护液相色谱柱、提高柱效。随着SPE硅胶小柱填料量的增加，CLE测定值减小，使用填料规格为0.5 g的SPE硅胶小柱可以得到较好的分离及富集效果。SPE硅胶小柱预处理所得物经超高效液相色谱-质谱联用分析证实为CLE。SPE可有效提取富集亚麻籽油所含的CLE，适用于HPLC定量检测CLE的前处理，该方法样品加标回收率为92.62%，组内精密度相对标准偏差为0.62%，组间精密度相对标准偏差为1.79%。 |
| 英文摘要: |
| The purification and enrichment effects of solvent extraction method and solid phase extraction(SPE) method on the quantitative determination of bitter peptide(CLE) in flaxseed oil by HPLC were compared. Furthermore, the pretreatment effects of SPE silica gel column with different filler specifications were compared. The results showed that the flaxseed oil pretreated by the solvent extraction method and the SPE method was quantitatively determined by HPLC, and the CLE could be well separated, and the pretreatment methods did not affect the peak time and peak shape of the CLE. However, compared with the solvent extraction method, triglyceride and other impurities in cyclolinopeptide sample extracted by the SPE method significantly decreased, which was extremely advantageous for protecting the chromatography column and improving the column efficiency. With the increase of the filler amount of SPE silica gel column, the CLE measurement value decreased. A good separation and enrichment effect could be obtained by using a SPE silica gel column with a filler amount of 0.5 g. The results of UPLC-MS analysis of SPE silica gel column pretreatment showed that it was indeed CLE. The SPE method could effectively extract CLE from flaxseed oil, and it was suitable for pretreatment of HPLC quantitative determination of CLE. The recovery of standard addition of the method was 92.62%, and the RSDs of the precision within the group and between the groups were 0.62% and 1.79% respectively. |
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