超声萃取-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 the contents of 23 Kinds of Phthalate Plasticizers in Leather and Leather Products by Ultra-high Performance Liquid Chromatography/Orbitrap High Resolution Mass Spectrometry Coupled with Ultrasonic Extraction

作　　者：王成云[1] 廖文忠[1] 李燕华[1] 施钦元[1] 钟声扬[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：《皮革与化工》2016年第3期5-12,共8页Leather And Chemicals

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/Orbitrap HRMS）方法,该方法以正己烷为萃取溶剂,超声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/Orbitrap HRMS分析,外标法定量。目标分析物的分离在Hypersil GOLD色谱柱（100 mm×2.1 mm×1.9μm）上进行,流动相为甲醇/0.1%甲酸溶液（含5 mmol/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80.9%～96.2%,相对标准偏差（RSD）为2.8%～10.2%（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,可完全满足皮革及其制品中邻苯二甲酸酯类增塑剂含量检测工作的需要。An effective method was established for the simultaneous determination of the contents of23 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 ultrasonically extracted using n-hexane as the extraction solvent.Then the extracts were purified by Al-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 ofmethanol and 0.1% aqueous formic acid solution containing 5 mmol/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 phthalate 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 80.9% to 96.2% while the relative standard deviation（RSD） changed from 2.8% to 10.2%（n=9）. The limits of detection（LODs） varied from 0.1μg/kg to 2.0μg/kg. The method was rapid, simple, sensitive and accurate, which could completely satisfy the demand on the determination of phthalate plasticizers in leather and leather products.

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

分 类 号：O657.63[理学—分析化学] TS57[理学—化学]