Benetti C, Piro R, Binato G, Angeletti R, Biancotto G
Istituto Zooprofilattico Sperimentale delle Venezie, Viale dell'Università, 10, I-35020, Legnaro (PD), Italy.
Food Addit Contam. 2006 Nov;23(11):1099-108. doi: 10.1080/02652030600699338.
A sensitive and specific method based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), for the simultaneous determination of lincomycin and five macrolide antibiotics in honey, was developed and validated. The analytes were extracted with Tris buffer 0.1 M, pH 10.5, and cleaned-up by a single solid-phase extraction step on OASIS HLB column. The chromatographic separation of analytes was performed on a Synergi Hydro-RP reversed-phase column using a gradient programme of aqueous 0.01 M ammonium acetate, pH 3.5, and acetonitrile as the mobile phase, at a flow rate 0.25 ml min-1. The detection of analytes was achieved by positive ionization electrospray in multiple reaction-monitoring mode. Two characteristic transitions were monitored for each substance. The following analytical parameters were validated according to the guidelines laid down by European Commission Decision 2002/657/EC (European Commission 2002): linearity, specificity, decision limit (CCalpha), detection capability (CCbeta), repeatability, within-laboratory reproducibility, recovery and ruggedness.
建立并验证了一种基于高效液相色谱-串联质谱(HPLC-MS/MS)的灵敏且特异的方法,用于同时测定蜂蜜中的林可霉素和五种大环内酯类抗生素。分析物用0.1 M、pH 10.5的Tris缓冲液萃取,并通过在OASIS HLB柱上进行单一固相萃取步骤进行净化。分析物的色谱分离在Synergi Hydro-RP反相柱上进行,使用0.01 M乙酸铵水溶液(pH 3.5)和乙腈作为流动相的梯度程序,流速为0.25 ml min-1。通过正离子电喷雾在多反应监测模式下实现分析物的检测。每种物质监测两个特征性跃迁。根据欧盟委员会第2002/657/EC号决定(欧盟委员会,2002年)规定的指南,对以下分析参数进行了验证:线性、特异性、决策限(CCα)、检测能力(CCβ)、重复性、实验室内再现性、回收率和耐用性。