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目的:测定多抗原肽MAP4原料药中醋酸及三氟乙酸的残留量。方法:采用反相高效液相色谱法,采用十八烷基硅烷键合硅胶为填充剂的Kromasil(250mm×4.6mm,10μm),200色谱柱;pH3.0磷酸盐缓冲液及甲醇为流动相,进行梯度洗脱;检测波长:210nm;柱温为25℃;流速:0.8ml/min;进样体积:40μl。结果:该方法中醋酸和三氟乙酸的分离度符合要求;醋酸的检测限0.1μg;三氟乙酸的检测限0.1μg;样品中未检出三氟醋酸。醋酸含量为5.7%。结论:该方法快速,准确,专属性强,精密度高,对多抗原肽MAP4原料药的质量控制有一定的意义。
OBJECTIVE: To determine the residues of acetic acid and trifluoroacetic acid in the multi-antigen peptide MAP4 drug substance. METHODS: Kromasil (250 mm × 4.6 mm, 10 μm) column 200 using octadecylsilane bonded silica gel as the mobile phase was used for reversed-phase high-performance liquid chromatography. Phosphate buffer 3.0 and mobile phase methanol , Gradient elution; detection wavelength: 210nm; column temperature of 25 ℃; flow rate: 0.8ml / min; injection volume: 40μl. Results: The separation of acetic acid and trifluoroacetic acid was satisfactory. The detection limit of acetic acid was 0.1μg and the detection limit of trifluoroacetic acid was 0.1μg. Trifluoroacetic acid was not detected in the sample. Acetic acid content of 5.7%. Conclusion: The method is rapid, accurate, specific and precise. It is of great significance to the quality control of multi-antigen peptide MAP4.