Sanders P, Delépine B
Ministère de l'Agriculture et de la Forêt, Unité de Pharmacocinétique, La Haute Marche, Fougeres, France.
Biol Mass Spectrom. 1994 Jun;23(6):369-75. doi: 10.1002/bms.1200230612.
To ensure that residues of veterinary drugs, above their respective maximum residue limits, do not reach the human food supply, European Community regulations specify requirements for detection, quantification and confirmation analytical methods and control procedures. The European Community member states base meat controls on these protocols. A liquid chromatographic/mass spectrometric analysis of spiramycin in calf muscle is presented as a confirmatory method for this compound. A particle beam interface was used, with negative ion chemical ionization mass spectrometry, using methane as the reagent gas. Samples (2 g muscle were prepared by liquid/liquid extraction followed by solid-phase extraction clean-up. On-line liquid chromatography/mass spectrometry of extracts was carried out on a C-18 bonded silica column. The specificity required for a regulatory confirmation procedure was achieved by monitoring five fragment ions with m/z 304, 330, 475, 683 and 684. Variation of the relative ion abundances was less than 20% at the maximum limit of residue, 50 micrograms kg-1. The method specificity was tested for three related compounds: neospiramycin, erythromycin and tylosin. The detection limit based on ion chromatogram peaks areas obtained with control samples was determined to be 20 micrograms kg-1.
为确保兽药残留量不超过各自的最大残留限量，从而不进入人类食品供应体系，欧盟法规对检测、定量和确证分析方法以及控制程序做出了规定。欧盟成员国的肉类控制措施均基于这些协议。本文介绍了一种用于检测小牛肌肉中螺旋霉素的液相色谱/质谱分析法，作为该化合物的确证方法。采用粒子束接口，以甲烷作为反应气，进行负离子化学电离质谱分析。样品（2 g肌肉）经液/液萃取，再通过固相萃取净化。提取物的在线液相色谱/质谱分析在C-18键合硅胶柱上进行。通过监测m/z为304、330、475、683和684的五个碎片离子，实现了监管确证程序所需的特异性。在最大残留限量50微克/千克时，相对离子丰度的变化小于20%。对三种相关化合物：新螺旋霉素、红霉素和泰乐菌素进行了方法特异性测试。根据对照样品获得的离子色谱峰面积确定检测限为20微克/千克。
