Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Athens 15771, Greece.
Talanta. 2012 Aug 15;97:32-41. doi: 10.1016/j.talanta.2012.03.058. Epub 2012 Apr 24.
This work reports a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for identification and quantification of seven sulfonamides, trimethoprim and dapsone in honey. The method is based on a solid-phase extraction (SPE) step of the target analytes with Oasis HLB cartridges after acidic hydrolysis of the honey sample to liberate the sugar-bound sulfonamides. Analysis was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive electro-spray ionization (ESI) mode with two different isotopically labeled internal standards with the view to improve the quantitative performance of the method. The method validation has been performed according to the Commission Decision 2002/657/EC; the average recoveries, measured at three concentration levels (1.5, 2.5 and 5.0 μg kg(-1)), have been estimated in the range 70 to 106% while the respective % relative standard deviations of the within-laboratory reproducibility ranged from 6 to 18%. Mean values of the expanded uncertainties calculated were in the range 22-41% at the 99% confidence level. Decision limit (CCα) and detection capability (CCβ) values were in the ranges 0.4-0.9 and 0.7-1.4 μg kg(-1), respectively. Matrix effects have been investigated demonstrating a moderate signal suppression/enhancement for most of the target compounds. The method described has been successfully applied to the analysis of honey samples; sulfamethoxazole, sulfathiazole and trimethoprim were detected in some cases.
本工作报道了一种灵敏的液相色谱-串联质谱（LC-MS/MS）方法，用于鉴定和定量蜂蜜中的七种磺胺类药物、甲氧苄啶和氨苯砜。该方法基于固相萃取（SPE）步骤，在酸性水解蜂蜜样品以释放糖结合的磺胺类药物后，用 Oasis HLB 小柱提取目标分析物。采用液相色谱-串联质谱（LC-MS/MS）在正电喷雾电离（ESI）模式下进行分析，使用两种不同的同位素标记内标，以提高方法的定量性能。该方法验证符合欧盟委员会 2002/657/EC 决定；在三个浓度水平（1.5、2.5 和 5.0 μg kg(-1))下测量的平均回收率估计在 70%至 106%之间，而实验室内部重现性的相应%相对标准偏差范围为 6%至 18%。在 99%置信水平下计算的扩展不确定度的平均值在 22%-41%范围内。决策界限（CCα）和检测能力（CCβ）值分别在 0.4-0.9 和 0.7-1.4 μg kg(-1)范围内。已研究了基质效应，证明大多数目标化合物存在中等程度的信号抑制/增强。所描述的方法已成功应用于蜂蜜样品的分析；在某些情况下检测到磺胺甲恶唑、磺胺噻唑和甲氧苄啶。
