高效液相色谱-串联质谱法测定贝类产品中31 种全氟及多氟烷基化合物含量

Determination of 31 kinds of perfluoroalkyl and polyfluoroalkyl substances content in aquatic products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法（HPLC-MS/MS）  全氟化合物（PFASs）  水产品  QuEChERS方法  检出限。

英文关键词:high performance liquid chromatography-tandem mass spectrometry  perfluoroalkyl and polyfluoroalkyl substances  aquatic products  QuEChERS

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定贝类产品中的31种全氟及多氟烷基化合物(perfluoroalkyl and polyfluoroalkyl substances, PFASs)含量的方法。方法 对贝类产品中31种PFASs的提取采用乙腈超声振荡提取, 选用QuEChERS方式净化, 加入氯化钠、无水硫酸镁、N-丙基乙二胺(N-propyl ethylenediamine, PSA)粉净化分层后, 将上层提取液于45 ℃水浴氮吹至干后, 用流动相定容, 确定最优的前处理条件。采用高效液相色谱-串联质谱仪电喷雾离子源(electrospray ionization, ESI)负离子模式扫描, 多反应检测模式对PFASs进行检测, 通过优化离子源温度、喷雾电压及碰撞能量等仪器参数, 外标法定量, 建立高效液相色谱-串联质谱法测定31种PFASs的分析方法。结果 针对31种PFASs构建的标准曲线范围为0.02~20.00 ng/mL, 呈现出良好的线性关系, 加标回收实验结果表明, 31种PFASs的检出限为0.01~0.50 μg/kg, 回收率范围为70.3%~116.2%。结论 该方法前处理简单, 操作简便, 分析准确, 可以达到对贝类产品种31种PFASs化合物的检测分析。

英文摘要:

      Objective To develop a method for the determination of 31 kinds of perfluoroalkyl and polyfluoroalkyl substances (PFASs) content in aquatic products by high performance liquid chromatography-tandem mass spectrometry. Methods The extraction of 31 kinds of PFASs in aquatic products was conducted by ultasonic oscillation with acetonitrile, and the purification was selected by QuEChERS method. After adding sodium chloride, anhydrous magnesium sulfate, and N-propyl ethylenediamine (PSA) powder to purify and separate, the upper layer of the extraction solution was nitrogen-dried at 45 ℃ water bath until dry, and then it was diluted a constant volume with mobile phase to determine the optimal pretreatment conditionshe mobile phase was used to determine the volume, and the optimal pretreatment conditions were determined. Using high performance liquid chromatography-tandem mass spectrometry with electrospray ionization (ESI) in negative ion mode scanning and multiple monitoring mode to detect PFASs, the analytical method for the determination of 31 kinds of PFASs by high performance liquid chromatography-tandem mass spectetry was established by optimizing the instrument parameters such as ion source temperature, spray voltage and collision energy, and the standard addition method was used for quantitative analysis. Results The experimental resulted showed that the standard curve range constructed for 31 kinds of PFASs was 0.02–20.00 ng/mL, exhibiting a good linear relationship. The spiked recovery experiment results showed that the limits of detection of 31 kinds of PFASs were 0.01–0.50 μg/kg, and the recovery rate ranges were 70.3%–116.2%. Conclusion This method has simple preprocessing, easy operation, accurate analysis, and can achieve the detection and analysis of 31 kinds of PFAS compounds in aquatic species.