Analysis of four polycyclic aromatic hydrocarbons in plant-based food supplements—results of a collaborative study

The determination of carcinogenic polycyclic aromatic hydrocarbons (PAHs) in food supplements is challenging, especially due to the presence of other e.g. heterogeneous PAH-like compounds in the matrix. A collaborative study with 12 participants was conducted in order to assess performance characteristics of a fast method intended to analyse the four regulated PAHs (PAH 4) benzo[b]fluoranthene [BbF], benz[a]anthracene [BaA], chrysene [CHR] and benzo[a]pyrene [BaP] in five different plant-based food supplements in the form of capsules, powder, and tablets. The principle of the method includes the extraction of PAHs with ethyl acetate: cyclohexane followed by a two-step SPE cleanup and final analysis by GC-MS or LC-FLD. The regulated maximum level for BaP is 10 µg/kg and, for the PAH 4, 50 µg/kg. Accordingly, the method was validated for the regulated PAH 4 analytically challenging concentration range from 2.5 µg/kg to 6.9 µg/kg. The performance criteria for the method set in European Regulation No 333/2007 for the overall repeatability, reproducibility (HorRat values below 2), and recovery (range 50–120%) were fulfilled. Based on the statistical evaluation of the results, it was concluded that the method is a suitable alternative to existing methods and should be studied for additional matrices.

食品补充剂中致癌性多环芳烃（polycyclic aromatic hydrocarbons, PAHs）的检测颇具挑战，尤其是基质中存在其他诸如异质性类多环芳烃类化合物时。本研究联合12家参与单位开展，旨在评估一种快速检测方法的性能特征：该方法可针对涵盖胶囊、粉剂、片剂三种剂型的5种不同植物基食品补充剂中的4种管控多环芳烃（PAH 4）——苯并[b]荧蒽（benzo[b]fluoranthene, BbF）、苯并[a]蒽（benz[a]anthracene, BaA）、䓛（chrysene, CHR）以及苯并[a]芘（benzo[a]pyrene, BaP）进行分析。该方法的原理为：以乙酸乙酯-环己烷混合溶剂萃取多环芳烃，随后经两步固相萃取（Solid Phase Extraction, SPE）净化，最终通过气相色谱-质谱联用（GC-MS）或液相色谱-荧光检测器（LC-FLD）完成分析。欧盟相关管控标准中，苯并[a]芘（BaP）的最大残留限量为10 µg/kg，PAH 4的总限量为50 µg/kg。据此，本方法针对PAH 4的分析挑战性浓度区间（2.5 µg/kg至6.9 µg/kg）完成了方法学验证。本方法满足欧盟第333/2007号法规设定的全部性能判据：总重复性、复现性（贺维茨比值HorRat小于2）以及回收率（50%~120%范围）均符合要求。基于对实验结果的统计评估，本方法可作为现有检测方法的合适替代方案，建议针对更多基质类型开展进一步研究。