QuEChERS⁃气相色谱⁃串联质谱法测定木制食品接触材料中五氯苯甲醚含量

Determination of pentachloroanisole content in wooden food contact materials by QuEChERS-gas chromatography-tandem mass spectrometry

中文关键词:  五氯苯甲醚  食品接触材料 QuEChERS气相色谱串联质谱

英文关键词:pentachloroanisole  food contact materials  QuEChERS-gas chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS?气相色谱?串联质谱法测定木制食品接触材料中五氯苯甲醚的分析方法。方法 制备的样品中加纯水和二氧化锆球超声, 接着依次加入溶剂乙腈和盐包(硫酸镁和氯化钠)振荡、离心, 上层提取溶剂经分散固相萃取净化后, 氮吹至近干, 加正己烷振荡复溶, 经0.22 μm微孔滤膜过滤后, 采用DB-5MS石英毛细管色谱柱(30 m×0.25 mm, 0.25 μm)分离, 在电子轰击离子源和多反应监测模式下检测, 外标法定量。结果 五氯苯甲醚在0.2~10.0 μg/L质量浓度内呈良好的线性关系(r2=0.999)。定量限为0.5 μg/kg, 检出限为0.2 μg/kg。木制样品添加3个浓度水平的五氯苯甲醚, 每个浓度水平6个平行, 测定的回收率为85.3%~97.4%, 相对标准偏差为3.0%~3.6%。结论 该方法操作简便、具有较高的灵敏度、特异度和精确性, 适用于木制食品接触材料中五氯苯甲醚的测定。

英文摘要:

      Objective To establish a method for the determination of pentachloroanisole in wooden food contact materials by QuEChERS-gas chromatography-tandem mass spectrometry. Methods The prepared samples were added with pure water and zirconia beads, followed by ultrasonic extraction. Acetonitrile and a salt package (magnesium sulfate and sodium chloride) were sequentially added, and the mixture was shaken and centrifuged. The upper extract was purified by dispersive solid-phase extraction, concentrated to near dryness under nitrogen flow, redissolved by shaking with n-hexane, and filtered through a 0.22 μm microporous membrane. Separation was performed on a DB-5MS quartz capillary column (30 m×0.25 mm, 0.25 μm), and detection was carried out using an electron ionization source in multiple reaction monitoring mode. Quantification was achieved by the external standard method. Results Pentachloroanisole showed a good linear relationship in the concentration range of 0.2–10.0 μg/L (r2=0.999). The limit of quantitation was 0.5 μg/kg, and the limit of detection was 0.2 μg/kg. Wooden samples were spiked with pentachloroanisole at 3 concentration levels, with 6 replicates at each level. The recoveries ranged from 85.3% to 97.4%, and the relative standard deviations were 3.0%–3.6%. Conclusion The method is simple to operate, with high sensitivity, specificity and precision, and is suitable for the determination of pentachloroanisole in wooden food contact materials.