压延烘干法制备用于定量分析的叠氮硝胺吸收药

为缩短叠氮硝胺吸收药组分定量分析时间,采用压延烘干法制备了样品,并与过筛烘干法制备的样品进行了比较。用液相色谱法、卡尔·费休法分别检测了两种样品的组分含量和水分含量。结果表明,压延烘干法制备样品共需要1.2h,明显少于过筛烘干法的4.5h。压延烘干法制得的样品均匀性更好,使得取样量可以由过筛烘干法的2g减少到0.2g,配制试样溶液时所需的溶剂体积减少了90%。压延烘干后的样品含水质量分数为0.06%~0.12%,低于过筛烘干法制备的样品。表明用压延烘干法制备样品,可以减少样品组分定量分析的总时间,并且可以减少废溶剂量。

Azidonitramine Intermediate Sample Preparation for Quantitative Analysis by Calendering-drying Method

To shorten the quantitative analysis time of azidonitramine intermediate component, the samples were prepared by calendering-drying method, and was compared with the sample prepared by sieving-drying method.The component content and water content of samples from two preparation methods were detected respectively by liquid-chromatography and Karl-fischer method.The results show that the calendering-drying method requires 1.2h, much less than 4.5h of sieving-drying method.The uniformity of sample by calendering-drying method is better, making the amount of sample decrease from 2g of original method to 0.2g, and the solvent volume needed to make up sample solution can be reduced 90%.The mass fraction of water in the samples prepared after calendaring-drying is from 0.06% to 0.12%, lower than that in the samples prepared by sieving-drying method.The calendering-drying method to prepare the azidonitramine intermediate sample can shorten the whole quantitative analysis time, and reduce the waste solution dose.