UPLC-MS/MS测定二苯甲烷二异氰酸酯

Determination of Diphenylmethane Diisocyanate by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了二苯甲烷二异氰酸酯（MDI）的超高效液相色谱-串联质谱（UPLC-MS/MS）联用的分析方法。实验用甲醇作衍生试剂,将二苯甲烷二异氰酸酯衍生成二苯甲烷二氨基甲酸甲酯（MDC）,通过测定二苯甲烷二氨基甲酸甲酯来确定二苯甲烷二异氰酸酯的含量。实验采用Waters Acquity BEH C18超高效液相色谱柱,甲醇-0.1%甲酸作为梯度洗脱液,二苯甲烷二氨基甲酸甲酯在1.5 min内与其他化合物进行完全分离,经四极杆质谱选择离子监测模式检测。线性范围为2~100μg/L,检出限为1μg/L,相关系数0.999 4。考察了水、甲酸、甲酸铵流动相体系,以及进样量大小对样品的分离效果,发现甲酸流动相体系的分离效果优于其他两种流动相体系,同时发现在进样量大时出现平头峰。并且在优化条件下,对实际样品中游离的二苯甲烷二异氰酸酯进行了测定。

A sensitive ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） method was developed for the separation and determination diphenylmethane diisocyanate（MDI）.Methanol was used for the derived reagent,and diphenylmethane diisocyanate was transformed into diphenylmethane dicarbamate（MDC）,then calculated the content of MDI.The sample was effectively separated in 1.5 min on a Waters Acquity BEH C18 column using methanol and water（containing 0.1% formic） as mobile phase under the condition of gradient elution.The detection of compound was performed by MS under single ion monitoring（SIM） mode.The calibration curve is linear over the concentration range of 2—100 μg/L for the compound with detection limits of 1 μg/L,and the correlation coefficient is 0.999 4.The effects of mobile phase systems and the injection volumes of the sample were investigated.The results indicate that the separation efficiency of compounds in acidity mobile phase is higher than other systems,and the large injection has flat head peak in spectrum.Under the optimum conditions,the method was applied in the determination of free monomeric isocyanates in the actual samples.