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

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（100 mm×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0.2 μg/kg，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。

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

An effective method of ultra performance liquid chromatography-orbitrap high resolution mass spectrometry (UPLC-Orbitrap HRMS) was established for the simultaneous determination 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 acetonitrile 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.