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高效液相色谱/串联质谱法快速测定牛奶中的 9 种磺胺类药物,无需固相萃取。

Rapid method for quantification of nine sulfonamides in bovine milk using HPLC/MS/MS and without using SPE.

机构信息

Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain.

出版信息

Food Chem. 2013 Dec 1;141(3):2294-9. doi: 10.1016/j.foodchem.2013.04.099. Epub 2013 May 10.

Abstract

Sulfonamides are antimicrobial agents widely employed in animal production and their residues in food could be an important risk to human health. In the dairy industry, large quantities of milk are monitored daily for the presence of sulfonamides. A simple and low-cost extraction protocol followed by a liquid chromatographic-tandem mass spectrometry method was developed for the simultaneous detection of nine sulfonamides in whole milk. The method was validated at the maximum residue limits established by European legislation. The limits of quantification obtained for most sulfonamides were between 12.5 and 25 μg kg(-1), detection capabilities ranged from 116 to 145 μg kg(-1), and recoveries, at 100 μg kg(-1), were greater than 89±12.5%. The method was employed to analyse 100 raw whole bovine milk samples collected from dairy farms in the northwest region of Spain. All of the samples were found to be compliant, but two were positive; one for sulfadiazine and the other for sulfamethoxipyridazine.

摘要

磺胺类药物是一种广泛应用于动物生产的抗菌剂,其在食品中的残留可能对人类健康构成重要威胁。在乳制品行业,每天都要对大量牛奶进行磺胺类药物残留检测。本研究建立了一种简单、低成本的提取方法,并结合液相色谱-串联质谱法,用于同时检测全脂牛奶中的 9 种磺胺类药物。该方法的验证符合欧洲法规规定的最大残留限量。大多数磺胺类药物的定量限在 12.5-25μg/kg 之间,检测限在 116-145μg/kg 之间,在 100μg/kg 添加水平下的回收率大于 89±12.5%。该方法用于分析了来自西班牙西北部地区的 100 份生牛乳的原始样本,所有样本均符合要求,但有 2 个样本呈阳性,一个样本中检出磺胺嘧啶,另一个样本中检出磺胺二甲氧嘧啶。

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