Institute of Quality Standard & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, PR China; Key Laboratory of Agro-product Quality and Safety, Ministry of Agriculture, Beijing 100081, PR China.
Institute of Quality Standard & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, PR China; Key Laboratory of Agro-product Quality and Safety, Ministry of Agriculture, Beijing 100081, PR China.
J Chromatogr A. 2019 Dec 20;1608:460423. doi: 10.1016/j.chroma.2019.460423. Epub 2019 Aug 14.
In order to address the specific question of food safety in livestock and poultry, it is imperative to monitor veterinary drugs at every moment in the process of livestock and poultry breeding. Thus, multi-residue analysis of a wide variety of drugs using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has become a tool of critical significance, especially for veterinary drug monitoring programs. A total of 160 compounds, belonging to 17 different families of veterinary drugs, were investigated in the urine and blood of livestock and poultry. Drug samples were extracted using a slightly acidic acetonitrile solution. The QuEChERS (quick, easy, cheap, effective, rugged, and safe) preparation method, combined with dispersive solid phase extraction (d-SPE) was compared with the approach of solid phase extraction (SPE). In the end, the QuEChERS extraction procedure was selected to reduce matrix effects and efficiently extract target veterinary drugs, and d-SPE was applied as a cleanup step. Electrospray ionization coupled with positive dynamic multiple reaction monitoring (dMRM) was utilized for the analysis of 160 different drugs in a single chromatographic run of 24 min. The efficiency of this method was evaluated using 7 matrices (pig blood, cattle blood, sheep blood, chicken blood, pig urine, cattle urine, and sheep urine). Good linearity was obtained for the analytes in a concentration range of 1-100 ng/mL, with correlation coefficients higher than 0.990. Most of the 160 drugs studied gave estimated limits of detection (LOQs) of 1 ng/mL, with some LOQs reaching as much as 5 ng/mL. The mean recoveries at four spike-in levels of 1, 5, 10, and 50 ng/mL, ranged from 60% to 120%. The intra-day precision measurements had coefficients of variation (n = 6) <15%, and the inter-day precision measurements were below 25%. Our method was applied in real samples and proved to be adequate for routine analysis. The proposed method proved to be simple, rapid and reliable for monitoring 160 drugs in the urine and blood of livestock and poultry, and can also be used for food safety monitoring.
为了能够解决有关畜禽食品安全的具体问题，在进行畜禽养殖时必须对兽药进行实时监控。因此，使用超高效液相色谱-串联质谱法（UHPLC-MS/MS）对多种药物进行多残留分析已成为一种非常重要的手段，尤其是在兽药监测计划中。本研究共检测了来自 17 个不同兽药家族的 160 种化合物在畜禽尿液和血液中的残留情况。采用弱酸性乙腈溶液提取药物样本。QuEChERS（快速、简单、廉价、有效、耐用、安全）提取法与固相萃取法（SPE）相比，结合分散固相萃取（d-SPE）具有更大的优势。最终选择 QuEChERS 提取程序以降低基质效应并有效提取目标兽药，然后应用 d-SPE 作为净化步骤。采用电喷雾正离子动态多重反应监测（dMRM），在 24 分钟的单个色谱运行中分析了 160 种不同药物。该方法在 7 种基质（猪血、牛血、羊血、鸡血、猪尿、牛尿和羊尿）中进行了评估。分析物在 1-100ng/mL 的浓度范围内具有良好的线性关系，相关系数均大于 0.990。在所研究的 160 种药物中，大多数药物的估计检测限（LOQs）为 1ng/mL，有些 LOQs 低至 5ng/mL。在 1、5、10 和 50ng/mL 四个加标水平下的平均回收率范围为 60%-120%。日内精密度测量的变异系数（n=6）<15%，日间精密度测量的变异系数低于 25%。该方法应用于实际样品，结果证明该方法适用于常规分析。该方法简单、快速、可靠，可用于监测畜禽尿液和血液中的 160 种药物，也可用于食品安全监测。
