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    傅里叶变换红外光谱法测定吲哚美辛胶囊中滑石粉的含量

    Determination of Talc in Indomethacin Capsules by Fourier Transform Infrared Spectroscopy

    • 摘要: 为实现药品制剂中滑石粉含量的准确测定,提出了题示方法。取含滑石粉约5 mg的吲哚美辛胶囊内容物,置于已于450 ℃恒重的瓷坩埚内,在500 ℃加热板上碳化30 min,再于450 ℃炽灼至恒重。取约一半质量的残渣和100 mg溴化钾,在玛瑙研钵中研磨5 min,分取约50 mg,在压力40 kN下压片3 min,采用傅里叶变换红外光谱仪测量(669±2)cm−1处滑石粉特征吸收峰的吸光度,并根据吸光度和滑石粉质量分数间的线性定量关系计算样品中滑石粉的含量。结果显示:滑石粉的线性范围为0.5%~3.5%,检出限为0.05%;对滑石粉对照品片和样片进行精密度试验,吸光度的相对标准偏差(n=6)均不大于4.0%;按照标准加入法进行回收试验,回收率为101%~110%。方法用于7个企业87批吲哚美辛胶囊样品的分析,在4个企业生产的样品中检出了滑石粉,检出量为1.90~12.70 mg·粒−1,与企业提供的处方量不符,且在3个企业生产的样品中存在明显的批次间差异。

       

      Abstract: In order to achieve the accurate determination of talc in pharmaceutical preparations, the method mentioned by the title was proposed. Contents of indomethacin capsules containing about 5 mg of talc were taken, and placed into a porcelain crucible with constant weight at 450 ℃, carbonized at 500 ℃ heating plate for 30 min, and then incandesced at 450 ℃ to constant weight. About half of the residue and 100 mg of potassium bromide were taken, and ground in an agate mortar for 5 min. About 50 mg of the mixture was taken, and pressed into a pellet at pressure of 40 kN for 3 min. The absorbance of the characteristic absorption peak of talc at (669±2) cm−1 was measured by Fourier transform infrared spectrometer, and the content of talc in the sample was calculated according to the linear quantitative relationship between the absorbances and mass fractions of talc. It was shown that the linear range of talc was 0.5%‒3.5%, with the detection limit of 0.05%. RSDs (n=6) of absorbance was less than 4.0% for talc reference pellets and sample pellets. Test for recovery was made according to the standard addition method, giving the recovery in the range of 101%‒110%. The proposed method was applied to the analysis of 87 batches of indomethacin capsule samples from 7 enterprises. Talc was detected in the samples produced by 4 enterprises, and the detection amount was 1.90‒12.70 mg·capsule−1, which was inconsistent with the prescription amount provided by the enterprises, and there were significant differences between batches in the samples produced by 3 enterprises.

       

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