Department of Analytical Chemistry, University of Barcelona, Diagonal 647, E-08028 Barcelona, Spain.
Anal Chim Acta. 2011 Jan 10;683(2):227-33. doi: 10.1016/j.aca.2010.10.034. Epub 2010 Nov 3.
In this study, an automated on-line solid-phase extraction coupled to fast liquid chromatography-tandem mass spectrometry (on-line SPE fast LC-MS/MS) method was developed for the simultaneous analysis of bisphenol A (BPA), bisphenol F (BPF), bisphenol E (BPE), bisphenol B (BPB) and bisphenol S (BPS) in canned soft drinks without any previous sample treatment. A C18 (12 μm particle size) loading column was used for the SPE on-line preconcentration before the liquid chromatography baseline separation of bisphenol compounds using a C18 Fused-Core™ (50 mm × 2.1 mm i.d.) column, which took less than 3 min. Gradient elution and heated electrospray were used to reduce matrix effect and improve ionization efficiency. To select the most intense and selective transitions, fragmentation studies were performed by multiple-stage mass spectrometry in an ion trap mass analyzer and tandem mass spectrometry in a triple quadrupole instrument, this latter instrument being used for quantitation in SRM mode. Quality parameters of the method were established and we obtained a simple, fast, reproducible (RSD values lower than 10%) and accurate (precision higher than 93%) method for the analysis of bisphenols in canned soft drinks at the ng L(-1) level using matrix-matched calibration.
本研究建立了一种无需样品前处理的全自动在线固相萃取-快速液相色谱-串联质谱法（在线 SPE 快速 LC-MS/MS），用于同时分析罐装软饮料中的双酚 A（BPA）、双酚 F（BPF）、双酚 E（BPE）、双酚 B（BPB）和双酚 S（BPS）。采用 C18（12μm 粒径）装填柱进行在线 SPE 预浓缩，然后在 C18 融合核（50mm×2.1mm i.d.）柱上进行双酚化合物的液相色谱基线分离，整个过程耗时不到 3 分钟。采用梯度洗脱和加热电喷雾，以降低基质效应并提高离子化效率。为了选择最强和最具选择性的离子，通过离子阱质谱仪中的多级质谱碎裂研究和三重四极杆仪器中的串联质谱进行碎裂研究，后者用于基质匹配校准的 SRM 模式定量。该方法的质量参数得到了确立，我们获得了一种简单、快速、重现性好（RSD 值低于 10%）、准确（精度高于 93%）的方法，可用于分析罐装软饮料中的双酚，检测限达到 ng L(-1)水平。
