超高效液相色谱-静电场轨道阱高分辨质谱法同时测定合成革中8种异氰酸酯残留  

Simultaneous determination of the residues of eight isocyanates in synthesized leathers using ultra performance liquid chromatography-orbitrap high resolution mass spectrometry

作　　者：王成云[1] 李丽霞[1] 林君峰[1] 褚乃清[1] 谢堂堂[1] 

机构地区：[1]深圳出入境检验检疫局工业品检测技术中心,广东深圳518067

出　　处：《色谱》2016年第9期888-894,共7页Chinese Journal of Chromatography

基　　金：国家质检总局科研项目(2014IK163)~~

摘　　要：建立了超高效液相色谱-静电场轨道阱高分辨质谱（UPLC-Orbitrap HRMS）同时测定合成革中8种异氰酸酯残留的方法.样品中残留的异氰酸酯经二氯甲烷超声萃取后,用9-甲氨基甲基蒽（ MAMA）进行衍生,衍生产物浓 缩定容后进行UPLC-Orbitrap HRMS分析,外标法定量.衍生产物在Hypersil GOLD色谱柱（100mm×2. 1 mm, 1.9 μm）上进行分离,流动相为乙腈-0. 1%（ v/v）甲酸水溶液,采用电喷雾正离子（ ESI＋ ）模式电离,以保留时间和 准分子离子精确质量数定性,以提取离子色谱峰面积定量.各组分的定量限均为0.2μg/k g,在3个加标浓度水平下,方法的平均加标回收率为85. 41% - 95. 53%,相对标准偏差（ RSD ）为 2. 55% - 6. 87%.应用该方法对市售合成革产品进行监测,结果在1个样品中检出了异佛尔酮二异氰酸酯.该方法定性准确,定量限低,灵敏度高,可用于合成革中异氰酸酯残留的测定.An effective method of ultra performance liquid chromatography-orbitrap high reso-lution mass spectrometry （UPLC-Orbitrap HRMS） was established for the simultaneous deter-mination of the residues of eight isocyanates in synthesized leathers. Residual isocyanates in synthesized leathers were ultrasonically extracted using dichloromethane as the extraction solvent and derivatized by 9-（ methylaminomethyl） anthracene （MAMA） at the same time. The derivatives were concentrated and analyzed by UPLC-Orbitrap HRMS technique. The concentration of each analyte was calibrated by the external standard method. The derivatives were separated on a Hypersil GOLD column （100 mm×2. 1 mm, 1. 9 μm） with a gradient elution of aceto-nitrile and 0. 1% （v/v ） formic acid aqueous solution, and analyzed by Orbitrap HRMS in positive ESI mode. The qualitative analyses were carried out by the exact masses of quasi-molecular ions and the retention times. The quantitative analyses were carried out by the peak areas in extracted chromatograms. The limits of quantification （LOQs） were 0. 2 μg/kg for all the eight isocyanates. The analytes were spiked in blank samples at three levels and the average recoveries varied from 85. 41% to 95. 53% with the relative standard deviations （RSDs） of 2. 55%-6. 87%. The proposed method was applied in the analysis of synthesized leather products and isophorone diisocyanate （IPDI） was detected in a real sample. The proposed method was accurate and sensitive, and applicable to the determination of the residues of isocyanates in synthesized leathers.

关 键 词：超高效液相色谱 静电场轨道阱高分辨质谱 异氰酸酯 合成革 

分 类 号：O658[理学—分析化学]