甲醇衍生-高效液相色谱法快速定量分析1,5-萘二异氰酸酯

Rapid Quantitative Analysis of 1,5-Naphthalene Diisocyanate Product by Methanol Derivative-High Performance Liquid Chromatography

针对1，5-萘二异氰酸酯（NDI）对水活泼的特性，采用甲醇为衍生试剂与NDI发生衍生化反应，利用高效液相色谱法结合紫外检测器测定非光气法制备NDI反应过程中产物的含量．通过对NDI标准品的衍生产物进行质谱分析测试，证实标准品衍生化后可得到高纯度的甲醇衍生产物．液相色谱条件为：采用AgilentHC-Cx8（250mm×4．6mm，5pm）色谱柱，以甲醇一水为流动相进行等度洗脱，流速为1．0mL／min，柱温35℃，紫外检测波长为220nm，进样量10μL．结果表明：本方法的线性相关系数大于0．999，检出限为0．0128mg／L（信噪比为3），平均加标回收率为97．99％～99．55oA（n=6）之间，相对标准偏差为0．71％～1．40％．本方法简单快速，准确度高，可用于工业NDI产物的定量分析．

A derivatization reaction of methanol derivative reagent with 1,5-naphthalene diisocyanate （NDI） was applied because of the NDI which was actively to water easily. NDI product content in the reac- tion process by non-phosgene method was determined by the high performance liquid chromatography with ultraviolet absorbance detector （UV）. The compositions of the NDI product after derivatization were examined by the mass spectrometric analysis, and confirmed that the high purity methanol derivatives could be obtained after derivatization. The conditions of high performance liquid chromatography were as follows. An Agilent HC-Cls （250 mm×4.6 mm, 5 /μm）column was used for the separation at the column temperature of 35 ℃ Isocratic elution was employed with a mobile phase consisting of methanol and water with a flow rate of 1.0 μL/min. The detection wavelength was 220 nm and the injection volume was 10 gL. The results showed that the method has a good linear correlation with the correlation coefficients above 0. 999. The de- tection limit was 0. 012 8 mg/L （S/N=3）, and the average recoveries were 97.99%~99.55% （n=6） with relative standard deviations of 0.71 N ~ 1.40N. The method is simplew fast, accurate, and can be used to quantitative analysis of industrial NDI product.