Departamento de Química, Unidad Departamental de Química Analítica, Facultad de Ciencias, Universidad de La Laguna (ULL), San Cristóbal de La Laguna, Spain.
Consiglio Nazionale delle Ricerche (CNR), Istituto per i Sistemi Biologici (ISB), Rome, Italy.
Electrophoresis. 2020 Oct;41(20):1768-1775. doi: 10.1002/elps.202000032. Epub 2020 May 14.
The separation of 11 phthalic acid ester (PAEs) was carried out by nano-liquid chromatography coupled to ultraviolet and MS detection. Preliminary experiments were achieved in order to select suitable stationary phases and chromatographic conditions. The baseline separation was obtained, for all compounds, with an XBridge C column in less than 15 min, working in step gradient mode. The sensitivity of the method was improved by on-column focusing. PAEs were extracted from alcoholic and nonalcoholic beverages using vortex-assisted emulsification dispersive liquid-liquid microextration and natural deep eutectic solvents. The whole method was validated in terms of linearity, sensitivity, precision, recovery, and repeatability. Combination of both off-line sample preparation preconcentration and large injection volume led to obtain LOQs in the range 5-47 ng/mL. The developed nano-LC-UV method was extended to MS detection to confirm the presence of PAEs in some beverages commercialized in different types of packaging.
采用纳米液相色谱法与紫外和质谱检测联用的方法对 11 种邻苯二甲酸酯（PAEs）进行了分离。初步实验旨在选择合适的固定相和色谱条件。所有化合物均在不到 15 分钟内，采用 XBridge C 柱，在分步梯度模式下实现了基线分离。通过柱上聚焦提高了方法的灵敏度。采用涡旋辅助乳化分散液液微萃取和天然深共晶溶剂从酒精和非酒精饮料中提取 PAEs。从线性、灵敏度、精密度、回收率和重复性等方面对整个方法进行了验证。离线样品制备浓缩和大进样量的组合使 LOQs 在 5-47ng/mL 的范围内。将开发的纳米 LC-UV 方法扩展到 MS 检测，以确认在不同包装类型的市售饮料中存在 PAEs。
