National Reference Laboratory of Veterinary Drug Residues (SCAU), College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Oct 1;936:10-7. doi: 10.1016/j.jchromb.2013.07.028. Epub 2013 Aug 7.
A simple multiresidue method was developed for detecting and quantifying twenty analytes from 5 classes of prohibited veterinary drugs (β-agonists (9), anabolic hormones (4), quinoxalines (4), tranquilizers (1), cyproheptadine, and clonidine in animal feeds using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach. Feed samples were extracted by ultrasonic-assisted extraction with a mixture of methanol-acetonitrile (50:50, v/v), followed by a cleanup using a dispersive solid-phase extraction with PSA (primary secondary amine). Target compounds were separated and determined by a liquid chromatography tandem quadrupole mass spectrometer operating in positive electrospray ionization mode, using multiple reaction monitoring (MRM). The recoveries of these compounds were between 56.7% and 103% at three spiked levels. The repeatability was lower than 10%, whereas reproducibility was no more than 15% except for nandrolone (17% at 10μgkg(-1)) and diazepam (19% at 10μgkg(-1)). Decision limits (CCαs) and detection capabilities (CCβs) ranged from 0.42 to 5.74μgkg(-1) and 5.70-9.81μgkg(-1), respectively. The method was successfully applied to screening of real samples obtained from local feed markets and confirmation of the suspected target analytes.
建立了一种简单的多残留方法,用于检测和定量分析动物饲料中 5 类禁用兽药(β-激动剂(9)、同化激素(4)、喹恶啉类(4)、镇静剂(1)、赛庚啶和可乐定)中的 20 种分析物。采用 QuEChERS(快速、简单、廉价、有效、坚固和安全)方法,通过甲醇-乙腈(50:50,v/v)混合超声辅助提取,再用 PSA(伯仲胺)分散固相萃取进行净化,提取饲料样品。目标化合物采用正电喷雾电离模式的液相色谱串联四极杆质谱仪,通过多反应监测(MRM)进行分离和测定。这些化合物在三个加标水平的回收率在 56.7%到 103%之间。重复性低于 10%,除了去甲雄三烯醇酮(10μgkg(-1)时为 17%)和地西泮(10μgkg(-1)时为 19%)外,重现性不超过 15%。决策限(CCαs)和检测能力(CCβs)分别为 0.42-5.74μgkg(-1)和 5.70-9.81μgkg(-1)。该方法成功应用于当地饲料市场获得的实际样品的筛选,并对可疑目标分析物进行了确认。