衰减全反射傅立叶变换红外光度法快速测定西甲硅油中二甲硅油的含量

Rapid determination of dimethicone in simethicone by ATR-FT-IR spectrophotometry

目的:建立衰减全反射傅里叶变换红外(ATR-FT-IR)光度法快速测定西甲硅油中二甲硅油含量。方法:采用标准曲线法,以液体石蜡为溶剂,测定二甲硅油质量分数在10%~100%范围内的标准曲线,继而测定西甲硅油中二甲硅油的含量。扫描次数为32次,扫描范围为4000~525 cm^-1,分辨率为4 cm^-1,测定二甲硅油的红外特征吸收峰为1260 cm^-1处,量取峰高作为吸收度。采用本文的快速测定方法和现行方法同时测定同一批样品的二甲硅油含量,检验差异性。结果:二甲硅油质量分数在10%~100%范围,与吸收度呈良好的线性关系(r=0.9995),3个浓度模拟样品的平均回收率为100.6%,RSD(n=6)为0.34%;6批样品的含量测定结果为94.4%、94.6%、94.2%、94.7%、94.2%、94.5%;通过采用2个正态总体的方差齐性检验法的F值检验法和t值检验法发现本文的快速测定方法和现行方法测定结果无显著性差异。结论:本方法简便、快捷且环保,准确度高、精密度好,优于以往的方法,可用于西甲硅油中二甲硅油含量的快速测定。

Objective:To establish a Fourier transform infrared spectrophotometry with attenuated total reflection(ATR-FT-IR)for assay of dimethicone in simethicone.Methods:The content of dimethicone in simethicone was calculated by standard curve using paraffin oil as solvent.The spectra were recorded 32 times scan each measure,in the range from 4000 cm^-1 to 525 cm^-1 with resolution of 4 cm^-1.The characteristic wavenumber of 1260 cm^-1 was selected for determination and the peak height was used as absorbance value.The content of dimethicone in simethicone was determined both by the rapid method proposed and current standard method,measuring the difference between these two methods.Results:There was a good linearity between mass fraction and absorbance value(r=0.9995),in the range of 10%-100%,the average recovery of three concentrations of simulation samples was 100.6% with RSD(n=6)of 0.34%.The content results of 6 batches of samples were 94.4%,94.6%,94.2%,94.7%,94.2%,94.5%.F-value Test and t-value Test were used to test homogeneity of variance between the two methods.The results showed that there was no significant difference between the two methods.Conclusion:The established method is simple,rapid and environmentally friendly,with high accuracy and precision.It is suitable for determination of dimethicone in simethicone.