微波辅助萃取-超高效液相色谱/静电场轨道阱高分辨质谱法同时测定皮革及其制品中23种邻苯二甲酸酯类增塑剂的含量  

Simultaneous Determination of 23 Kinds of Phthalate Plasticizers in Leather and Leather Products by Ultra-high Performance Liquid Chromatography/Orbitrap High Resolution Mass Spectrometry Combined with Microwave-assisted Extraction

作　　者：王成云[1] 张伟亚[1] 李燕华[1] 钟声扬[1] 林君峰[1] WANG Cheng-yun ZHANG Wei-ya LI Yan-hua ZHONG Sheng-yang LIN Jun-feng(The Testing and Technology Center for Industrial Products, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, China)

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：《西部皮革》2016年第13期37-43,共7页West Leather

基　　金：国家质检总局科研项目(2014IK163)

摘　　要：建立了同时测定皮革及其制品中23种邻苯二甲酸酯类增塑剂含量的超高效液相色谱／静电场轨道阱高分辨质谱（UPLC／OrbitrapHRMS）方法，该方法以乙腈为萃取溶剂，微波萃取皮革及其制品中的邻苯二甲酸酯类增塑剂，萃取液经中性氧化铝固相萃取柱净化后，进行UPLC／OrbitrapHRMS分析，外标法定量。目标分析物的分离在HypersilGOLD色谱柱（100mm×2．1min×1．9μm）上进行，流动相为甲醇／0．1％甲酸溶液（含5mmol／L乙酸铵），电离模式为电喷雾正离子（ESI＋），利用保留时间和准分子峰的精确质量数进行定性，利用提取色谱峰面积进行定量。23种邻苯二甲酸酯类增塑剂在其线性范围内均有良好的线性关系，线性相关系数均大于0．997，方法的加标平均回收率为80．3％-95．6％，相对标准偏差（RSD）均小于10％（n=9），检出限为0．1-2．0μg／kg。该方法简单快速，灵敏度高，检出限低，为开展皮革及其制品中邻苯二甲酸酯类增塑剂水平的调查与监测提供了技术支持。An effective method was established for the simultaneous determination of the contents of 23 kinds of phthalate plasticizers in leather and leather products using ultra-high performance liquid chromatography/orbitrap mass spectrometry （UPLC/Orbitrap） technique. Phthalate plasticizers in leather and leather products were microwave-assisted extracted using acetonitrile as the extraction solvent. Then the extracts were purified by A1-N solid phase extraction column, followed by the analysis of ultra-high performance liquid chromatography/orbitrap mass spectrometry （UPLC/Orbitrap）. The concentration of each analyte was calibrated by the external standard method. Phthalate plasticizers were separated on a Hypersil GOLD column （100 mm× 2.1 mm×1.9μm） with a gradient elution of methanol and 0.1% aqueous formic acid solution containing 5mmol/L ammonium acetate, and then detected by orbitrap high resolution mass spectrometry in ESI positive ion mode. The qualitative analysis was carried out by the retention time of phtha- late plasticizers and the accurate mass of each quasimolecular ion. The quantitative analysis was carried out by the peak area in extracted chromatogram with accurate mass. As to 23 kinds of phthalate plasticizers, good linear relationships existed in their concentration ranges with the correlation coefficients （r） more than 0.997. The spiked average recoveries varied from 80.3% to 95.6% while the relative standard deviation （RSD） all less than 10% （n=9）. The limits of detection （LODs） varied from0.1μg/kg to 2.0μg/kg. The method was rapid, simple, sensitive and accurate, and provided the basis for the investigation and monitoring of the levels of ph- thalate plasticizers in leather and leather products.

关 键 词：皮革 邻苯二甲酸酯类增塑剂 超高效液相色谱/静电场轨道阱高分辨质谱 微波辅助萃取 

分 类 号：TS57[轻工技术与工程—皮革化学与工程]