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目的:建立小样本量(<1 mL)预混精蛋白重组人胰岛素注射液的效价检测方法,并进行相关的方法学验证。方法:采用C18柱(Phenomenex,4.6 mm×250 mm,5μm);流动相为0.2 mol.L-1硫酸盐缓冲液-乙腈(73∶27);检测波长为214 nm;流速1.0 mL.min-1;柱温40℃。结果:重组人胰岛素溶液在6 h内稳定性良好,低、中、高浓度组的加样回收率分别为96.7%,97.0%,96.7%,小样本量法与大样本量法(即中国药典规定方法)检测同批次预混精蛋白重组人胰岛素注射液效价,结果无显著区别。结论:本文建立的小样本量法适用于评价单只预混精蛋白重组人胰岛素笔芯及使用中笔芯的实际效价,对检测具有重要的实用价值。
OBJECTIVE: To establish a method for the determination of the titer of pre-mixed protamine recombinant human insulin injection (<1 mL) and to verify the methodologies. Methods: C18 column (Phenomenex, 4.6 mm × 250 mm, 5 μm) was used. The mobile phase consisted of 0.2 mol·L-1 sulfate buffer and acetonitrile (73:27). The detection wavelength was 214 nm and the flow rate was 1.0 mL min- 1; column temperature 40 ℃. RESULTS: The recombinant human insulin solution had good stability within 6 h, and the recovery rates of the recombinant human insulin solution were 96.7%, 97.0% and 96.7% respectively. The small sample size method and large sample size method (ie, Chinese Pharmacopoeia Prescribed method) to detect the same batch of pre-mixed recombinant human insulin injection titer, the results no significant difference. Conclusion: The small sample size method established in this paper is suitable for the evaluation of the actual titer of single pre-mixed concentrate human insulin refill and the refill used, which is of great practical value for testing.