The present work presents a novel and rapid analytical method for the simultaneous analysis of bisphenol A (BPA), bisphenol B (BPB), bisphenol F (BPF) and bisphenol S (BPS) in edible oil based on dispersive micro solid phase extraction (DMSPE) for the first time followed by isotope dilution-ultra high performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS). The edible oil sample was dispersed by n-hexane and extracted with ammoniated methanol-water solution. Then the target analytes were dispersedly absorbed using the polymer anion exchange (PAX) as the sorbent and eluted by acidic methanol. After that, four bisphenols were separated on a C18 column by gradient elution with methanol and 0.05% ammonium hydroxide in water as mobile phase, detected by MS/MS under multiple reactions monitoring (MRM) mode and quantified by internal standard method. The PAX amounts, adsorption time, concentrations of formic acid in the elution solvent and volume of elution solvent for the DMSPE technique were optimized. The limit of detection and quantitation (LOD and LOQ), matrix effect, recovery and precision of the developed method were investigated. Results indicated that BPS and the rest three bisphenols displayed excellent linearity in the concentration ranges of 0.1–50 μg/L and 0.5–250 μg/L, respectively, with correlation coefficients (R²) all larger than 0.998. Achieved MLODs (S/N = 3) varied between 0.1–0.4 μg/kg for all bisphenols. The mean recoveries at three spiked levels in edible oil were in the range of 87.3–108%. Intra-day precision (n = 6) and inter-day precision (n = 5) were <9% and <11%, respectively. This method is of rapid-and-simple pretreatment, accurate and sensitive, and suitable for the simultaneous determination of bisphenols in edible oil.

本工作提出了一种基于分散微固相萃取（DMSPE）同时分析食用油中双酚A（BPA），双酚B（BPB），双酚F（BPF）和双酚S（BPS）的新颖，快速的分析方法），然后进行同位素稀释-超高效液相色谱串联质谱分析（UPLC–MS / MS）。食用油样品被n分散己烷，并用氨化的甲醇水溶液萃取。然后，使用聚合物阴离子交换剂（PAX）作为吸附剂将目标分析物分散吸收，并用酸性甲醇洗脱。此后，在C18色谱柱上通过以甲醇和0.05％氢氧化铵水溶液为流动相进行梯度洗脱，分离出四种双酚，在多反应监测（MRM）模式下通过MS / MS进行检测，并通过内标法进行定量。优化了DMSPE技术的PAX量，吸附时间，甲酸在洗脱溶剂中的浓度以及洗脱溶剂的体积。研究了所开发方法的检测限和定量限（LOD和LOQ），基质效应，回收率和精密度。R ²）均大于0.998。 对于所有双酚，达到的MLOD（S / N = 3）在0.1–0.4μg/ kg之间。食用油中三个加标水平的平均回收率在87.3–108％的范围内。日内精度（n  = 6）和日间精度（n  = 5）分别为<9％和<11％。该方法预处理快速，简便，准确，灵敏，适用于同时测定食用油中双酚的含量。