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一种用于定量空气样品中双酚A的毛细管高效液相色谱/电喷雾串联质谱法的开发与验证

Development and validation of a capillary high-performance liquid chromatography/electrospray tandem mass spectrometric method for the quantification of bisphenol A in air samples.

作者信息

Sabatini Laura, Barbieri Anna, Violante Francesco Saverio

机构信息

Occupational Medicine Unit, University of Bologna, S. Orsola-Malpighi Hospital, via Palagi 9, 40138 Bologna, Italy.

出版信息

Rapid Commun Mass Spectrom. 2005;19(23):3468-72. doi: 10.1002/rcm.2221.

Abstract

Bisphenol A (BPA) is a toxic industrial chemical that affects the endocrine system even at low concentrations. A new method, based on capillary high-performance liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC/ESI-MS/MS) analysis, has been developed to determine BPA in atmospheric samples. The method involves collection of air samples (typically 2 m(3)) on glass fiber filters, with ultrasonic extraction and sample concentration under vacuum before analysis. HPLC analysis was performed isocratically at a flow rate of 10 microL min(-1) using a capillary reversed-phase column and MS/MS analysis in negative ion multiple reaction monitoring (MRM) mode, using BPA-d(16) as internal standard. The present method provides linear response in the range 0.007-3.5 microg/filter (R(2) > 0.999) and is characterized by high accuracy (mean bias 2%) and good reproducibility (mean RSD 5%). High sensitivity (LOD = 2 ng/m(3) based on 2 m(3) of air collected), specificity, and speed of the analysis make the present method suitable for routine determination of BPA in the atmosphere, both for ambient and personnel monitoring.

摘要

双酚A(BPA)是一种有毒的工业化学品,即使在低浓度下也会影响内分泌系统。一种基于毛细管高效液相色谱/电喷雾电离串联质谱(HPLC/ESI-MS/MS)分析的新方法已被开发出来,用于测定大气样品中的双酚A。该方法包括在玻璃纤维滤膜上采集空气样品(通常为2立方米),在分析前进行超声提取并在真空下浓缩样品。使用毛细管反相柱以10微升/分钟的流速进行等度HPLC分析,并在负离子多反应监测(MRM)模式下进行MS/MS分析,使用双酚A-d(16)作为内标。本方法在0.007 - 3.5微克/滤膜范围内提供线性响应(R(2) > 0.999),具有高精度(平均偏差2%)和良好的重现性(平均相对标准偏差5%)。高灵敏度(基于采集2立方米空气计算的检测限 = 2纳克/立方米)、特异性和分析速度使本方法适用于大气中双酚A的常规测定,无论是环境监测还是人员监测。

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