高效液相色谱-串联质谱法同时测定钓具涂层中4种游离二异氰酸酯

Simultaneous Determination of 4 Kinds of Free Diisocyanate Monomers in Fishing Tackle Coating by Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法同时测定钓具涂层中4种游离二异氰酸酯的检测方法。样品中游离的二异氰酸酯经甲醇超声萃取衍生,再经C18固相萃取柱净化后,采用高效液相色谱-串联质谱法进行分析,外标法定量。4种游离二异氰酸酯的衍生物在2~100μg/L范围内峰面积与质量浓度呈现良好线性关系,检出限为0.3~0.5μg/kg。回收率在3个添加水平下达91.9%~97.1%,相对平均偏差为2.1%~5.2%。利用该法对市售钓鱼竿涂层进行检测,结果在5个样品中检出二苯甲烷二异氰酸酯。该方法定性准确、检出限低、灵敏度高,可用于钓具涂层中游离二异氰酸酯的测定。

An effective method of liquid chromatography-tandem mass spectrometry was established for the simultaneous determination of 4 kinds of free diisocyanate monomers in fishing tackle coating.The free diisocyanate monomer in the sample were ultrasonically extracted and derivatized by methanol at the same time.After purification by C18 solid phase extraction column,analysis was carried out by liquid chromatography-tandem mass spectrometry and quantitative analysis was performed by external standard method.The four kinds of free diisocyanate derivatives had good linear relationships in the range of 2~100μg/L with the limits of detection were0.3~0.5μg/kg.The recoveries of 4 diisocyanate derivatives at 3 different spiked levels were 91.9%~97.1%,with the relative standard deviations were 2.1%~5.2%.The proposed method was applied in the analysis of fishing tackles and Diphenylmethane diisocyanate was detected in five real samples.The proposed method was accurate and sensitive,and applicable to the determination of free diisocyanate monomers in fishing tackle coating.