UPLC/Orbittrap HRMS法测定涂布纸中邻苯二甲酸酯类增塑剂  

UPLC/Orbitrap HRMS determination of phthalate plasticizers in coated papers

作　　者：王成云[1] 张伟亚[1] 李燕华[1] 廖清萍[1] 林镱琳 沈雅蕾[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：《中华纸业》2017年第6期36-41,共6页China Pulp & Paper Industry

基　　金：国家质检总局科研项目(2014IK163)

摘　　要：建立了1个同时测定涂布纸中多种邻苯二甲酸酯类增塑剂的超高效液相色谱-静电场轨道阱高分辨质谱(UPLC/Orbitrap HRMS)方法,该方法以丙酮为萃取溶剂,采用微波辅助萃取技术提取涂布纸中的邻苯二甲酸酯类增塑剂,提取液经处理后进行UPLC/Orbitrap HRMS分析,外标法定量。样品中目标分析物的分离在Hypersil GOLD色谱柱(100mm×2.1mm×1.9μm)上进行,流动相为甲醇/5mmol醋酸铵水溶液(含0.1%甲酸),电离模式为电喷雾正离子(ESI^+)模式,根据保留时间和准分子峰的精确质量数进行定性,用提取色谱峰面积进行定量,各组分的质量准确度小于3ppm。对于每种目标分析物,在一定质量浓度范围内,其提取色谱峰面积均与质量浓度线性相关,且线性相关系数均不小于0.997,检出限为0.1~2.0μg/kg。在3个不同浓度的加标水平下,方法的加标平均回收率为80.3%~93.4%,相对标准偏差(RSD,n=9)为2.7%~9.5%。该方法定性可靠,定量准确,灵敏度高。应用该方法监测市售涂布纸中邻苯二甲酸酯类增塑剂的含量水平,结果在部分样品中检出不同含量水平的多种邻苯二甲酸酯类增塑剂。An UPLC/Orbitrap HRMS method was established for the determination of phthalate plasticizers in coated papers. Phthalate plasticizers in coated papers were microwave-assisted extracted using acetone as the extraction solvent; then the extract was treated and analyzed by ultra-high performance liquid chromatography/Orbitrap high resolution mass spectrometry（UPLC/Orbitrap HRMS） technique. The concentration of each analyte was calibrated by the external standard method. The analysis was carried out on a Hypersil GOLD column（100mm×2.1mm×1.9μm） with a gradient elution of methanol and 5mmol/l ammonium acetate solution consisting of 0.1% aqueous formic acid, and then detected by orbitrap HRMS in ESI positive ion mode. The qualitative analysis was carried out by the retention time and the accurate mass of quasimolecur ion. The quantitative analysis was carried out by the peak area in extracted chromatogram with accurate mass. Phthalate plasticizers were routinely detected with mass accuracy below 3 ppm under the optimal conditions. Good linearity was achieved in the respective linear ranges for each phthalate plasticizers, with correlation coefficients higher than 0.997. The limits of detection（LODs） varied from 0.1μg/kg to 2.0μg/kg. The blank samples were spiked at three levels and the spiked average recoveries changed from 80.3% to 93.4% while the relative standard deviation changed from 2.7% to 9.5%. The proposed method was simple, accurate and sensitive. The proposed method was applied in the determination of phthalate plasticizers in coated papers available commercially and phthalate plasticizers at different content levels were detected in some samples.

关 键 词：微波辅助萃取 超高效液相色谱 静电场轨道阱高分辨质谱 涂布纸 邻苯二甲酸酯 

分 类 号：TS77[轻工技术与工程—制浆造纸工程] TS727.3