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目的:通过比较同规格不同生产厂家的色谱柱对胸腺法新有关物质测定结果的影响,对中国药典2010年版二部收录的胸腺法新有关物质测定法进行探索研究。方法:选用十八烷基硅烷键合硅胶为填充剂的色谱柱(4.6mm×250mm,5μm);流动相A:乙腈-水-磷酸(140:860:1);流动相B:乙腈-水-磷酸(250:750:1),采用梯度洗脱;流速:1.0mL/min;紫外检测波长:210nm;进样量:20μl;柱温:室温。结果:针对碱破坏样品,同规格不同厂家的色谱柱间测试结果存在明显差异。结论:在使用《中国药典》2010年版二部收录的胸腺法新有关物质检测项下检测方法,对胸腺法新及其制剂进行有关物质检查时,应先进行色谱柱的筛选。采用Thermo scientific Hypersil GOLD C18(250×4.6mm、5?m)、GRACE AlltimaHP C18(250×4.6mm、5μm)色谱柱检测,主峰与峰前邻近杂质峰的分离度好,结果准确可靠,可用于注射用胸腺法新有关物质的测定。
OBJECTIVE: To explore the new method of thymus assay, which was included in the 2010 edition of Chinese Pharmacopoeia (TCM), by comparing the effects of different columns of different manufacturers on the determination of new related substances in thymus. Methods: The column (4.6mm × 250mm, 5μm) with octadecylsilane bonded silica gel as filler was used. The mobile phase A was acetonitrile - water - phosphoric acid (140: 860: 1) - Phosphoric acid (250: 750: 1) using a gradient elution; flow rate: 1.0 mL / min; UV detection wavelength: 210 nm; injection volume: 20 μl; Results: There are obvious differences between the test results of different samples from different manufacturers for alkali damage samples. Conclusion: When using the detection methods of the thymus test under the Chinese Pharmacopoeia 2010 edition 2, the column should be screened for the thymus and its preparations. The separation of the main peak from the peak adjacent to the peak was good with the Thermo Scientific Hypersil GOLD C18 (250 × 4.6 mm, 5 μm) and GRACE AlltimaHP C18 (250 × 4.6 mm, 5 μm) columns. The results were accurate and reliable, Injection thymus method for the determination of related substances.