Office of Regulatory Affairs, Arkansas Regional Laboratory, U.S. Food and Drug Administration , 3900 NCTR Road, Jefferson, Arkansas 72079, United States.
Agilent Technologies , Life Sciences & Diagnostics Group, 121 Hartwell Avenue, Lexington, Massachusetts 02421, United States.
Anal Chem. 2017 Mar 21;89(6):3256-3260. doi: 10.1021/acs.analchem.6b04889. Epub 2017 Mar 2.
The use of veterinary drugs in honey bees for the prevention of infectious disease is ever increasing due to the spread of colony collapse disorder around the world. The United States Food and Drug Administration is concerned about the presence of these drugs residues in honey as they often lead to health concerns or potential antibiotic resistance. Currently there is a need for a rapid screening method for the detection of veterinary drugs in honey. Herein is a method that utilizes automated solid-phase extraction that is directly coupled to a mass spectrometer for the quantitative screening of 12 different regulated sulfonamides in honey. Identification of the residues was performed using tandem mass spectrometry (MS/MS) with a triple quadrupole mass spectrometer. The acquisition method developed for this analysis can extract with the automated solid-phase extraction system and analyze a single sample on the mass spectrometer in approximately 20 s, with minimal sample preparation. A target testing limit of 10 ng/g in honey for the sulfonamides was used based upon action limits set for other food commodities regulated by the United States Food and Drug Administration. A complete method validation procedure was conducted to evaluate the effectiveness of this quantitative screening method.
由于世界各地的蜂群崩溃症候群的传播，兽医药物在蜜蜂中被用于预防传染病的使用不断增加。美国食品和药物管理局担心这些药物残留存在于蜂蜜中，因为它们经常导致健康问题或潜在的抗生素耐药性。目前，需要一种快速的筛选方法来检测蜂蜜中的兽药。在此，介绍了一种利用自动化固相萃取直接与质谱仪联用的方法，用于定量筛选蜂蜜中的 12 种不同的受监管的磺胺类药物。使用串联质谱（MS/MS）和三重四极杆质谱仪进行残留鉴定。该分析方法的采集方法可以在大约 20 秒内通过自动化固相萃取系统提取并在质谱仪上分析单个样品，样品制备量最小。基于美国食品和药物管理局监管的其他食品商品的行动限值，蜂蜜中磺胺类药物的目标检测限为 10 ng/g。进行了完整的方法验证程序，以评估这种定量筛选方法的有效性。
