Animal Drugs Research Center, US Food and Drug Administration, Denver Federal Center, Bldg 20, W 6th Ave. and Kipling St., Denver, CO 80225, USA.
Rapid Commun Mass Spectrom. 2012 Dec 30;26(24):2854-64. doi: 10.1002/rcm.6414.
Veterinary drug residue analysis of meat and seafood products is an important part of national regulatory agency food safety programs to ensure that consumers are not exposed to potentially dangerous substances. Complex tissue matrices often require lengthy extraction and analysis procedures to identify improper animal drug treatment. Direct and rapid analysis mass spectrometry techniques have the potential to increase regulatory sample analysis speed by eliminating liquid chromatographic separation.
Flumequine, oxolinic acid, and nalidixic acid were extracted from catfish, shrimp, and salmon using acidified acetonitrile. Extracts were concentrated, dried onto metal sample wells, then rapidly desorbed (6 s) with an infrared diode laser for analysis by laser diode thermal desorption atmospheric pressure chemical ionization with tandem mass spectrometry (LDTD-MS/MS). Analysis was conducted in selected reaction monitoring mode using piromidic acid as internal standard.
Six-point calibration curves for each compound in extracted matrix were linear with r(2) correlation greater than 0.99. The method was validated by analyzing 23 negative samples and 116 fortified samples at concentrations of 10, 20, 50, 100, and 600 ng/g. Average recoveries of fortified samples were greater than 77% with method detection levels ranging from 2 to 7 /g. Three product ion transitions were acquired per analyte to identify each residue.
A rapid method for quinolone analysis in fish muscle was developed using LDTD-MS/MS. The total analysis time was less than 30 s per sample; quinolone residues were detected below 10 ng/g and in most cases residue identity was confirmed. This represents the first application of LDTD to tissue extract analysis. Published 2012. This article is a US Government work and is in the public domain in the USA.
肉和海鲜产品中的兽药残留分析是国家监管机构食品安全计划的重要组成部分，旨在确保消费者不会接触到潜在危险物质。复杂的组织基质通常需要冗长的提取和分析程序来识别不当的动物药物处理。直接和快速的分析质谱技术有可能通过消除液相色谱分离来提高监管样品的分析速度。
采用酸化乙腈从鲶鱼、虾和三文鱼中提取氟甲喹、氧氟沙星和萘啶酸。提取液浓缩后，干燥至金属样品孔中，然后用红外二极管激光快速解吸（6 秒），采用激光二极管热解吸常压化学电离串联质谱（LDTD-MS/MS）进行分析。采用吡咯米酸作为内标，以选择反应监测模式进行分析。
每种化合物在提取基质中的六点校准曲线均呈线性，r²相关系数大于 0.99。通过分析 23 个阴性样本和 116 个浓度为 10、20、50、100 和 600 ng/g 的加标样本验证了该方法。加标样本的平均回收率大于 77%，方法检测限范围为 2 至 7 /g。每个残留物获得了三个产物离子跃迁以鉴定每个残留物。
采用 LDTD-MS/MS 开发了一种快速分析鱼肉中喹诺酮类药物的方法。每个样品的总分析时间少于 30 秒；检测到的喹诺酮残留低于 10 ng/g，在大多数情况下，残留物的身份得到了确认。这代表了 LDTD 首次应用于组织提取物分析。发表于 2012 年。本文为美国政府的作品，在美国属于公有领域。
