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目的:建立近红外一致性检验方法,用于快速检查药品标准物质组合包装(西林瓶、胶塞、铝塑盖)的密闭性,进而保证国家药品标准物质的质量。方法:选择易引湿的溴化钾作为试验样品,使用积分球方法采集近红外漫反射光谱,以2名不同操作人员测定的未引湿样品光谱为参照光谱,谱图经矢量归一化、一阶导数和17点平滑处理后,在谱段5 326~4 825 cm~(-1)和4 632~4 377 cm~(-1)建立一致性检验模型,阈值设定为4。在检查西林瓶组合包装密闭性时,将分装有未吸水溴化钾样品且包装完好的玻璃瓶放入密闭92%RH的高湿环境中24 h后,测定其近红外光谱,带入一致性检验模型,通过比较待测光谱与参照光谱的差异来判断其是否引湿,即密闭性是否有问题。结果:应用所建立的一致性检验模型分别预测正常样品和模拟包装密闭性有问题的样品,结果与实际情况一致。结论:所建一致性检验模型可以对组合包装密闭性有问题的样品做出准确的判断,可用于药品标准物质筛选西林瓶、胶塞和组合包装工艺的验证。
OBJECTIVE: To establish a near-infrared conformance test method for rapid examination of the hermeticity of pharmaceutical standard substance combinations (vials, stoppers, aluminum-plastic caps) to ensure the quality of national drug reference materials. Methods: The potassium bromide which is easy to dehumidify was selected as the test sample, the near-infrared diffuse reflectance spectra were collected by the integrating sphere method, and the spectra of non-wetted samples measured by two different operators were taken as the reference spectra. The spectra were normalized by vectors. After the first derivative and 17-point smoothing, a consistency test model was established between 5 326 and 4825 cm -1 and 4 632 to 4 377 cm -1 in the spectral range, and the threshold value was set at 4. When inspecting the airtightness of the package, the near-infrared spectrum was measured and the near-infrared spectrum was measured after placing the well-packed glass bottles packed with non-absorbed potassium bromide samples in a sealed, high-humidity environment at 92% RH for 24 h Sexuality test model, by comparing the difference between the measured spectrum and the reference spectrum to determine whether it is wet, that is, whether there is a problem sealing. Results: The established consistency test model was used to predict the samples with normal and simulated packaging imperfections respectively. The results were consistent with the actual situation. Conclusion: The proposed consistency test model can make an accurate judgment on the samples with confined packing problems and can be used to validate the drug standard materials for screening of vials, stoppers and combination packaging process.