螺旋藻中多环芳烃类新风险QuEChERS方法实证分析

目的:本研究旨在系统建立螺旋藻中多环芳烃气相色谱质谱联用仪(GC-MS/MS)分析方法,实证分析螺旋藻中发现的多环芳烃类污染新风险.方法:采用正己烷作为提取剂,超声辅助提取2次,合并提取液经QuEChERS净化,氮吹浓缩过滤后测定.定性和定量:使用DB-5 MS毛细管色谱柱分离,多反应监测模式(MRM)结合基质匹配外标...

Empirical Analysis of QuEChERS Method for New Risks of Polycyclic Aromatic Hydrocarbons in Spirulina

Objective: The purpose of this study was to systematically establish a gas chromatography-mass spectrometry (GC-MS/MS) analysis method for polycyclic aromatic hydrocarbons in Spirulina, and empirically analyze the new risk of polycyclic aromatic hydrocarbons found in Spirulina. Method: The polycyclic aromatic hydrocarbons of the sample were extracted twice with n-hexane ultrasonically, purified by QuEChERS, and tested after being concentrated by nitrogen blowing. Qualitative and quantitative: Separation using DB-5 MS capillary chromatographic column, multiple reaction monitoring mode (MRM) combined with matrix-matched external standard method for analysis. Results: The recovery rate was 68.8%～101.9%, the relative standard deviation was 1.8%～8.4% (n=6), the correlation coefficient of the equation reached above 0.999 within the linear range of 1～32 ng/mL, and the limit of quantitative (LOQ) was 2 μg/kg. Polycyclic aromatic hydrocarbons were detected in all 69 commercially available Spirulina samples, with the content in the range of 2.4 μg/kg to 3491 μg/kg. Conclusion: The QuEChERS detection method for 15 polycyclic aromatic hydrocarbons in Spirulina established in this paper is fast, accurate and highly sensitive, and can provide scientific technical support for daily supervision. It is necessary to pay attention to the risk of polycyclic aromatic hydrocarbons in Spirulina products, and further identify the source of pollution to establish prevention and control measures.