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采用针对液相色谱-串联质谱法量身定制的混合固相萃取-沉淀技术测定血清中的双酚A、4-叔辛基苯酚和4-壬基苯酚。

Bisphenol A, 4-t-octylphenol, and 4-nonylphenol determination in serum by Hybrid Solid Phase Extraction-Precipitation Technology technique tailored to liquid chromatography-tandem mass spectrometry.

作者信息

Asimakopoulos Alexandros G, Thomaidis Nikolaos S

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimioupolis Zografou, 15771 Athens, Greece.

Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimioupolis Zografou, 15771 Athens, Greece.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Apr 1;986-987:85-93. doi: 10.1016/j.jchromb.2015.02.009. Epub 2015 Feb 16.

Abstract

A rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and optimized for the simultaneous determination of bisphenol A, 4-t-octylphenol and 4-nonylphenol in human blood serum. For the first time, the electrospray ionization (ESI) parameters of probe position, voltage potential, sheath gas flow rate, auxiliary gas flow rate, and ion transfer tube temperature were thoroughly studied and optimized for each phenol by a univariate approach. As a consequence, low instrumental limits of detection were reported, demonstrating at 0.2 ng/mL (in solvent matrix) excellent injection repeatability (RSD<14.5%) and a confirmation peak for all target phenols. Extraction and purification of serum was performed by the novel Hybrid Solid Phase Extraction-Precipitation Technology technique (Hybrid SPE-PPT). The limits of detection in human blood serum were 0.80, 1.3 and 1.4 ng/mL for BPA, 4-t-OP and 4-NP, respectively.

摘要

建立并优化了一种快速液相色谱-串联质谱(LC-MS/MS)方法,用于同时测定人血清中的双酚A、4-叔辛基酚和4-壬基酚。首次采用单变量方法,对每种酚类物质的电喷雾电离(ESI)参数,包括探头位置、电压、鞘气流量、辅助气流量和离子传输管温度进行了深入研究和优化。结果表明,仪器检测限较低,在0.2 ng/mL(在溶剂基质中)时,所有目标酚类物质均具有出色的进样重复性(RSD<14.5%)和确认峰。血清的提取和纯化采用新型混合固相萃取-沉淀技术(Hybrid SPE-PPT)。双酚A、4-叔辛基酚和4-壬基酚在人血清中的检测限分别为0.80、1.3和1.4 ng/mL。

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