目的：为组合化学合成结构相似小分子多肽提供快速准确的ＨＰＬＣ分析方法。方法：ＲｅｓｏｌｖＣ１８柱（５μｍ，４６ｍｍ×２００ｍｍ）。流动相：乙腈－水（２０∶８０），内含０１％三氟乙酸为流动相酸性调节剂。检测波长：２１４ｎｍ。结果：目标多肽纯度范围２６３６％～７７０２％，迁移时间２８９～３０１５ｍｉｎ。７号多肽纯度和迁移时间的ＲＳＤ分别为１９％和１４％。结论：应用本方法可快速准确分离分析结构相似的小分子多肽，尤其是组合化学合成的多肽。 OBJECTIVE: To provide a rapid and accurate HPLC analysis method for combinatorial chemical synthesis of structurally similar small molecule peptides. Method: Resolv C18 column (5 μm, 4  6 mm × 200 mm). Mobile phase: acetonitrile - water (20:80), containing 0.1% trifluoroacetic acid as mobile phase acidity regulator. Detection wavelength: 214nm. Results: The purity of target peptide ranged from 2636% to 7702%, and the migration time ranged from 289 to 3015min. The RSD of purity and migration time of peptide 7 were 19% and 14%, respectively. Conclusion: This method can be used to quickly and accurately separate and analyze small molecule peptides of similar structure, especially in combination with chemically synthesized peptides.