采用自制的全息平场凹面光栅集成微型光谱仪,搭建了微型光谱快速分析测试系统,实现了雷尼替丁合成中间体中杂质甲醛的快速检测。利用酸性条件下甲醛-MBTH-硫酸铁铵体系的显色作用,通过优化甲醛测定条件,建立了快速测定甲醛的方法。测定甲醛线性范围为0.04-0.20 μg·mL^-1(r=0.993 8),最低检测限达到0.04 μg·mL^-1。通过与UV-2550岛津光谱仪及美国海洋公司HR-2000微型光谱仪的对比测试实验,对所建立的微型光谱检测系统和甲醛检测方法进行了实际测试和可靠性验证,F-检验法检验显示测试结果无显著性差异。实验结果表明微型光谱快速分析测试系统能满足实验分析、工业过程监测和临床医学检验样品的快速、实时检测的需求,具有巨大的潜在应用市场。

The rapid and real-time analytical system based on photometrical methodology of a homemade holographic flat field concave grating integrated microspectrometer was established,which was applied to detect the remnant formaldehyde in the intermediate of ranitidine synthesis.Based on the chromogenic reaction of formaldehyde with MBTH and NH4Fe(SO4)2 in acid medium,the methodology of formaldehyde detection was developed.Furthermore,factors affecting the chromogenic reaction were optimized in details.Under the optimized conditions,a good linear relationship in the range of 0.04-0.20 μg·mL-1 (r=0.993 8) was obtained and the lowest detection limit achieved 0.04 μg·mL^-1.In order to demonstrate the methodology and reliability of the microspectrometer analytical system,comparative experiments were carried on among the homemade microspectrometer,SHIMADZU UV-2550 spectrophotometer and U.S.A.Ocean Optic HR2000 Microspectrometer.The F-test was employed to check the reliability and efficiency of the proposed methodology.No significant difference was shown among them.The experimental results showed that the set up analytical system could satisfy the needs of quick and real-time detection in practical applications for experimental analysis,industrial monitoring and medicinal diagnosis.