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| 高效增强除脂双层柱结合UPLC-MS/MS快速测定食品中23种全氟及多氟烷基化合物含量 |
| Determination of 23 kinds of PFASs in food by high efficiency reinforced fat removal bilayer column-ultra performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2025-02-17 修订日期：2025-06-26 |
| DOI： |
| 中文关键词: 全氟和多氟烷基化合物 高效增强除脂双层柱(HLB-P/HMR-Lipid) UPLC-MS/MS 食品 |
| 英文关键词:Per-and Polyfluoroalkyl Substances HLB-P/HMR-Lipid ultra performance liquid chromatography-tandem mass spectrometry food |
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| 中文摘要: |
| 目的? 建立高效增强除脂双层柱结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时检测食品中23种全氟和多氟有机化合物的分析方法。方法 样品经试样经提取、离心后，上清液经高效增强除脂双层柱的快速滤过式固相萃取柱净化后, 经Shim-pack GISS Hp 3 μm C18 ( 2.1 mm×150 mm，HSS)色谱柱分离, 以2 mmol/L甲酸铵水溶液和甲醇为流动相进行梯度洗脱, 质谱(ESI-)采用多反应监测模式(multiple response monitoring, MRM), 内标法定量。结果 23种目标化合物在色谱柱上有很好的保留, 在0.20~50.00 μg/L范围内具有良好线性(r2>0.995)。 当固体试样量为 2 g（精确至 0.001 g），液体试样 5 g（精确至 0.001 g），上机溶液定容体积为 0.2 mL 时，全氟丁烷羧酸（PFBA）和全氟戊烷羧酸（PFPeA）的检出限为 0.06 μg/kg、定量限为 0.18 μg/kg；剩余 21 种全氟化合物的检出限为0.03 μg/kg、定量限为 0.09 μg/kg。在猪肉、鱼肉和液态乳类基质样品中添加2.0 μg/kg和10.0 μg/kg 浓度水平的混合标准溶液做加标回收实验, 结果显示平均回收率为 70.3%~119%, 相对标准偏差(relative standard deviation, RSD)为 1.56%~9.65%。结论 该方法简单、快速、结果准确、灵敏度高, 适合测定食品中23种全氟和多氟烷基化合物。 |
| 英文摘要: |
| ABSTRACT: Objective To establish a method for simultaneous determination of 23 kinds of PFASs in food by high efficiency reinforced fat removal bilayer column-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods HLB-P/HMR-Lipid method was adopted for the purification, the sample solution was separated on an Shim-pack GISS Hp C18 column (2.1 mm×150 mm, 3 μm) using 2 mmol/L ammonium acetate and methanol were used as mobile phase for gradient elution, detected by MS/MS (ESI-) with multiple reactions monitoring (MRM), and quantified by internal standard method. Results In this method, 23 target compounds of PFASs were well retained on the chromatographic column with good linearity in the range of 0.20-50 μg/L (r2> 0.995). When the solid sample volume is 2.0 g (accurate to 0.001 g), the liquid sample is 5.0 g (accurate to 0.001 g), and the fixed volume of the machine solution is 0.20 mL, The limits of detection and quantification of PFBA and PFPeA were 0.06 μg/kg and 0.18 μg/kg respectively. The limits of detection and quantification of the remaining 21 perfluorinated compounds were 0.03 μg/kg and 0.09 μg/kg respectively. The recoveries of the 23 target compounds ranged from 69.8%~118% with relative standard deviations of 1.84%~11.6%. Conclusion This method is easy, fast, accurate and sensitive, which is suitable for the determination of 23 PFASs in food. |
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