Grupo de Investigación y Desarrollo en Química Analítica (QUIANID), LISAMEN-CCT-CONICET-Mendoza, Mendoza, Argentina.
J Agric Food Chem. 2011 Apr 27;59(8):3559-65. doi: 10.1021/jf104622x. Epub 2011 Apr 4.
A simple technique based on ultrasound-assisted emulsification microextraction in situ derivatization (USAEME-ISD) is proposed for the one-step derivatization, extraction, and preconcentration of bisphenol A (BPA) in beverage samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. BPA was in situ derivatized with acetic anhydride and simultaneously extracted and preconcentrated by using USAEME. Variables affecting the extraction efficiency of BPA were evaluated. Under optimal experimental conditions, the detection limit (LOD) was 38 ng L(-1) with a relative standard deviation (RSD) value of 11.6%. The linear working range was 100-1250 ng L(-1), and the coefficient of estimation (r(2)) of the calibration curve was ≥0.9971. The robustness of the proposed methodology was probed by developing a recovery study at two concentrations (125 and 500 ng L(-1)) over different beverage samples. This study led to a satisfactory result achieving recoveries of ≥82%, which showed acceptable robustness for determination of nanograms per liter of BPA in samples of food safety interest.
本文提出了一种基于超声辅助乳化微萃取原位衍生化（USAEME-ISD）的简单技术，用于在气相色谱-质谱（GC-MS）分析之前对饮料样品中的双酚 A（BPA）进行一步衍生化、提取和预浓缩。BPA 与乙酸酐就地衍生化，并通过 USAEME 同时提取和预浓缩。评估了影响 BPA 萃取效率的变量。在最佳实验条件下，检测限（LOD）为 38 ng L(-1)，相对标准偏差（RSD）值为 11.6%。线性工作范围为 100-1250 ng L(-1)，校准曲线的估计系数（r(2)）≥0.9971。通过在不同饮料样品中两种浓度（125 和 500 ng L(-1))进行回收研究来探测所提议方法的稳健性。该研究取得了令人满意的结果，回收率≥82%，这表明该方法在食品安全相关样品中测定纳克/升级别的 BPA 时具有可接受的稳健性。
