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短柱液相色谱-电喷雾电离串联质谱法测定牛奶中磺胺类抗生素的多残留量

Multiresidue determination of sulfonamide antibiotics in milk by short-column liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

作者信息

Volmer D A

机构信息

Institute for Marine Biosciences, National Research Council, Halifax, Nova Scotia, Canada.

出版信息

Rapid Commun Mass Spectrom. 1996;10(13):1615-20. doi: 10.1002/(SICI)1097-0231(199610)10:13<1615::AID-RCM747>3.0.CO;2-G.

Abstract

Liquid chromatography coupled to electrospray mass spectrometry and tandem mass spectrometry has been used for the determination and quantification of 21 sulfonamides and two potentiators (ormethoprim, trimethoprim) in milk. Separation using high-performance liquid chromatography was achieved in less than 6 min for all compounds on a short (4.0 x 50 mm, 3 micron) reversed-phase column. After sample clean-up, time-scheduled single-ion monitoring (SIM) yielded detection of sulfonamides in milk from low ppb level to the ppt level. The strategy used to detect, confirm and quantify sulfonamides in milk samples was as follows: (a) pre-screening (and cp3firmation) of target and non-target sulfonamides by precursor ion scan and/or multiple reaction monitoring experiments using generic product ions; (b) quantification of identified target compounds by monitoring their protonated molecule ions in a time-scheduled SIM experiment; (c) further confirmation, if necessary, by selected reaction monitoring using characteristic product ions.

摘要

液相色谱联用电喷雾质谱和串联质谱已用于测定和定量牛奶中的21种磺胺类药物和两种增效剂(奥美普明、甲氧苄啶)。使用高效液相色谱在短(4.0×50mm,3微米)反相柱上对所有化合物在不到6分钟内实现分离。样品净化后,定时单离子监测(SIM)可检测牛奶中低至十亿分之一(ppb)水平至万亿分之一(ppt)水平的磺胺类药物。用于检测、确认和定量牛奶样品中磺胺类药物的策略如下:(a) 通过使用通用产物离子的前体离子扫描和/或多反应监测实验对目标和非目标磺胺类药物进行预筛选(和确认);(b) 通过在定时SIM实验中监测其质子化分子离子对已鉴定的目标化合物进行定量;(c) 如有必要,通过使用特征产物离子的选择反应监测进行进一步确认。

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