Departamento de Química, ICEx, Universidade Federal de Minas Gerais, Belo Horizonte, 31270901, Brazil.
Departamento de Clínica, Patologia e Cirurgia Oral, Faculdade de Odontologia, Universidade Federal de Minas Gerais, Belo Horizonte, 31270901, Brazil.
Anal Bioanal Chem. 2020 Nov;412(28):7799-7810. doi: 10.1007/s00216-020-02908-x. Epub 2020 Aug 29.
Bisphenol A and phthalates are endocrine disruptors widely used as chemical additives mainly in plastic products, including materials for dentistry procedures. Besides, many plasticizers have been associated with important diseases requiring performed methods for their quantification. In the present study, an alternative method for the determination of bisphenol A (BPA) and phthalate metabolites in saliva was developed and validated using hollow fiber liquid phase microextraction (HF-LPME) for sample preparation and gas chromatography coupled to ion trap mass spectrometry (GC/MS) for analysis. A mixture of octanol and ethyl octanoate (1:1 v/v) was used as an acceptor phase in hollow fiber to extract the analytes from saliva samples. A Doehlert design was performed to optimize the variable sample agitation and extraction time. The HF-LPME-GC/MS method developed for saliva analysis showed good selectivity, linearity (R > 0.900), and precision (CV = 0.86-18.68%). Limits of detection and quantification ranged from 0.03 to 0.53 μg L and 0.09 to 1.78 μg L, respectively. A high concentration of BPA in the oral cavity and oropharyngeal space is a warning of the possible association with the main cancer of the mouth. The method developed and validated was applied to patients with oral squamous cell carcinoma (study group, n = 16) and patients who did not present any oral lesion (control group, n = 16). A principal component analysis was performed and showed a tendency for the association between oral squamous cell carcinoma (OSCC) and plasticizers. Graphical abstract.
双酚 A 和邻苯二甲酸酯是广泛用作化学添加剂的内分泌干扰物,主要用于塑料制品,包括牙科手术材料。此外,许多增塑剂与重要疾病有关,需要进行定量分析。在本研究中,开发并验证了一种替代方法,用于通过中空纤维液相微萃取 (HF-LPME) 进行样品制备和气相色谱-离子阱质谱联用 (GC/MS) 进行分析,以测定唾液中的双酚 A (BPA) 和邻苯二甲酸酯代谢物。辛醇和辛酸乙酯 (1:1 v/v) 的混合物被用作中空纤维中的接受相,从唾液样品中提取分析物。采用 Doehlert 设计优化了变量样品搅拌和提取时间。为唾液分析开发的 HF-LPME-GC/MS 方法表现出良好的选择性、线性 (R > 0.900) 和精密度 (CV = 0.86-18.68%)。检测限和定量限范围分别为 0.03-0.53 μg L 和 0.09-1.78 μg L。口腔和口咽空间中 BPA 的高浓度是可能与口腔主要癌症有关的警告。开发和验证的方法应用于口腔鳞状细胞癌患者 (研究组,n = 16) 和未出现任何口腔病变的患者 (对照组,n = 16)。进行了主成分分析,结果表明口腔鳞状细胞癌 (OSCC) 与增塑剂之间存在关联趋势。