Van Eeckhout N, Perez J C, Van Peteghem C
Laboratory of Food Analysis, Faculty of Pharmaceutical Sciences, Ghent University, Harelbekestraat 72, 9000 Ghent, Belgium.
Rapid Commun Mass Spectrom. 2000;14(24):2331-8. doi: 10.1002/1097-0231(20001230)14:24<2331::AID-RCM169>3.0.CO;2-J.
A sensitive, high performance liquid chromatography/tandem mass spectrometric (i.e. mass spectrometry/mass spectrometry; LC/MS/MS) method with on-line extraction and sample clean-up for the screening and confirmation of residues of sulfonamides in kidney is described. The sulfonamides are extracted from homogenized kidney with methanol. After centrifugation of the extract, an aliquot of the extract is directly injected on the LC/MS/MS system with further extraction and clean-up of the sample on-line. Detection of the analytes was achieved by positive electrospray ionization (ESI) followed by multiple reaction monitoring. For each sulfonamide the collisional decomposition of the protonated molecule to a common, abundant fragment ion was monitored. The method has been validated for sulfadimethoxine, sulfaquinoxaline, sulfamethazine, sulfamerazine, sulfathiazole, sulfamethoxazole, sulfadiazine and sulfapyridine. Calibration curves resulting from spiked blank kidney samples at the 10-200 microg/kg level showed good linear correlation. At the level of 50, 100 and 200 microg/kg both within- and between-day precision, as measured by relative standard deviation (RSD), were less than 16%. The limits of detection (LODs) ranged from 5 to 13.5 microg/kg. The recoveries ranged from 78 to 82%. The procedure provides a rapid, reliable and sensitive method for the determination of residues of sulfonamides in bovine kidney. The advantage of this method over existing methods is its decreased sample preparation and analysis time, which makes the method more suitable for routine analysis.
描述了一种用于筛查和确证肾脏中磺胺类药物残留的灵敏高效液相色谱/串联质谱法（即质谱/质谱；LC/MS/MS），该方法具有在线萃取和样品净化功能。磺胺类药物用甲醇从匀浆后的肾脏中萃取。萃取液离心后，取一份萃取液直接注入LC/MS/MS系统，同时在线对样品进行进一步萃取和净化。通过正电喷雾电离（ESI）和多反应监测实现对分析物的检测。对于每种磺胺类药物，监测质子化分子碰撞分解为常见的丰度较高的碎片离子的过程。该方法已针对磺胺二甲氧嘧啶、磺胺喹恶啉、磺胺二甲嘧啶、磺胺甲基嘧啶、磺胺噻唑、磺胺甲恶唑、磺胺嘧啶和磺胺吡啶进行了验证。在10 - 200μg/kg水平下，向空白肾脏样品中添加标准品得到的校准曲线显示出良好的线性相关性。在50、100和200μg/kg水平下，日内和日间精密度（以相对标准偏差（RSD）衡量）均小于16%。检测限（LOD）范围为5至13.5μg/kg。回收率范围为78%至82%。该方法为测定牛肾脏中磺胺类药物残留提供了一种快速、可靠且灵敏的方法。该方法相对于现有方法的优势在于减少了样品制备和分析时间，使其更适合常规分析。
