超高效液相色谱-串联质谱法同时测定青稞酒中多种类塑料添加剂

建立青稞酒中抗氧化剂、增塑剂、紫外线吸收剂、着色剂、表面活性剂和阻燃剂6个类别34个组分塑料添加剂的超高效液相色谱-串联质谱快速筛查检测方法。青稞酒样品中加水稀释至酒精度20%左右,盐析条件下用乙腈提取;色谱条件:Waters HSS T3 C_(18)柱(2.1 mm×150 mm,1.7μm),甲醇-0.1%乙酸铵为流动相梯度洗脱,流速为0.2 m L/min;串联质谱条件:以电喷雾离子源正离子模式电离,在多反应监测模式下分析;外标法定量。结果表明:34种塑料添加剂在较宽的质量浓度范围内线性关系良好,相关系数均大于0.99,两个添加量水平的回收率在71.2%~106.7%之间,精密度(相对标准偏差)在4.2%~15.4%之间,青稞酒中34种塑料添加剂的最低检出限为5~50μg/L。测定12批次青稞酒样品,共检出15种塑料添加剂。本方法适用于青稞酒中不同类别、物理和化学性质差异较大的多种类多组分塑料添加剂的定性确证、高灵敏度定量、快速筛查青稞酒中跨类别、多组分塑料添加剂。

Simultaneous Determination of Multiple Kinds of Plastic Additives in Highland Barley Liquor from Qinghai by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

The aim of study was to develop a novel method using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to determine 34 components, which are categorized into 6 kinds of plastic additives including antioxidant, plasticizer, ultraviolet light absorber, colorant, surfactant and fire retardant, in highland barley liquor. Samples were diluted with water to a 20% alcohol content, and extracted with acetonitrile under salting-out conditions. The UPLC system was equipped with a Waters HSS T3 C18 analytical column (2.1 mm × 150 mm, 1.7 μm) utilizing methanol-0.1% ammonium acetate as mobile phase in gradient elution mode with a ?ow rate of 0.2 mL/min. An electrospray ionization ion source under positive ion mode (ESI+) for multiple reaction monitoring analysis was used, and quantification was performed by an external standard method. The calibration curves exhibited a good linearity in wide concentration ranges with correlation coefficients of over 0.99 for all analytes. The average recoveries from spiked highland barley liquor at two concentrations ranged from 71.2% to 106.7% with relative standard deviations (RSDs) from 4.2% to 15.4%. The limits of detection (LODs) were between 5 and 50 μg/L. A total of fifteen kinds of plastic additives were found in 12 batches of samples. Therefore, the new method allowed simultaneous determination of different kinds of plastic additives that differ widely in physicochemical properties. It is a promising method for the identi?cation and quantitation of plastic additive compounds in liquor.