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采用高效薄层色谱法结合荧光密度法和电喷雾电离质谱检测技术快速、选择性测定多种磺胺类药物。

Rapid and selective determination of multi-sulfonamides by high-performance thin layer chromatography coupled to fluorescent densitometry and electrospray ionization mass detection.

机构信息

Institute of Food Chemistry, University of Hohenheim, Garbenstrasse 28, 70599 Stuttgart, Germany; School of Food Science and Technology, Jiangnan University, 214022 Wuxi, China.

Institute of Food Chemistry, University of Hohenheim, Garbenstrasse 28, 70599 Stuttgart, Germany.

出版信息

J Chromatogr A. 2014 Feb 28;1331:108-16. doi: 10.1016/j.chroma.2014.01.037. Epub 2014 Jan 24.

DOI:10.1016/j.chroma.2014.01.037
PMID:24507971
Abstract

In the European Union (EU), sulfonamides are among the most widely administrated groups of antibiotics in animal husbandry. Therefore, monitoring their residues in edible animal tissues plays an important role in the EU food safety framework. In this work, a simple and efficient method for the rapid screening of twelve prior sulfonamides frequently prescribed as veterinary drugs by high-performance thin-layer chromatography (HPTLC) was established. Sample extracts obtained with acetonitrile were tenfold concentrated and applied to HPTLC without any further cleanup. Following separation and fluram derivatization, sensitive and selective quantitation of the analytes can readily be accomplished with fluorescent densitometry. Limits of detection and quantitation were 15-40 and 35-70μg/kg, respectively. Additionally, a confirmative detection by HPTLC-electrospray ionization mass spectrometry (HPTLC-ESI/MS) was optimized, offering straightforward identification of target zones. Therefore, the risk of potential false positive findings can efficiently be reduced. The method was validated to meet the enforced commission regulation (EU) No. 37/2010, regarding different matrix complexities (bovine milk, porcine liver and kidney).

摘要

在欧盟(EU),磺胺类药物是畜牧业中使用最广泛的抗生素之一。因此,监测其在食用动物组织中的残留对于欧盟食品安全框架至关重要。在这项工作中,建立了一种简单高效的高效薄层色谱(HPTLC)快速筛选十二种常用于兽药的磺胺类药物的方法。用乙腈提取的样品提取物经十倍浓缩后,无需进一步净化即可应用于 HPTLC。分离和氟拉明衍生化后,用荧光密度法可轻松完成分析物的灵敏和选择性定量。检测限和定量限分别为 15-40 和 35-70μg/kg。此外,还优化了 HPTLC-电喷雾电离质谱(HPTLC-ESI/MS)的确认检测,可直接鉴定目标区域。因此,可以有效地降低潜在假阳性发现的风险。该方法经过验证,符合欧盟委员会法规(EU)No.37/2010 的要求,涵盖了不同基质复杂性(牛奶奶、猪肝和肾)。

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