The objective of this study was to optimize the analytical method for multi-class veterinary drug residues of 64 compounds in fishery products. Several compounds from veterinary drugs are banned or unauthorized in fishery products according to the Korean Food Code. Samples were extracted using acetonitrile/water (4:1, v/v) and the clean-up step was carried out by adding octadecylsilane and acetonitrile-saturated hexane. The target compounds were confirmed and quantified using liquid chromatography–tandem mass spectrometry (LC–MS/MS). The proposed method was validated according to the CODEX guidelines (CAC/GL-71), and most target compounds were found to be in acceptable quantities under the requirements of the validation guidelines. The recovery of analytes was typically in the 60–120% range, and precision, expressed as the coefficient of variation was less than 31% at all levels of concentration. The limit of quantification ranged from 0.03 to 3 μg kg−1 in the fishery products. Moreover, the application of the proposed method to 96 real samples demonstrated that no drug residues exceeded the Korean maximum residue limits (MRLs). This evaluation method provides reliable identification and quantification of multi-class veterinary drugs in fishery products and can be an efficient means to inspect drugs currently banned or not approved for aquaculture in Korea.

中文翻译：

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液相色谱-串联质谱法同时测定水产品中的多种兽药

这项研究的目的是优化水产品中64种化合物的多类兽药残留分析方法。根据《韩国食品法典》，在渔业产品中禁止或未经许可使用兽药中的几种化合物。使用乙腈/水（4：1，v / v）萃取样品，并通过添加十八烷基硅烷和乙腈饱和的己烷进行净化步骤。使用液相色谱-串联质谱法（LC-MS / MS）对目标化合物进行确认和定量。根据CODEX指南（CAC / GL-71）对提出的方法进行了验证，并且在验证指南的要求下，发现大多数目标化合物的含量都可以接受。分析物的回收率通常在60-120％的范围内，并且精密度，表示为在所有浓度水平下变异系数均小于31％。渔业产品中的定量限为0.03至3μgkg-1。此外，将拟议方法应用于96个真实样品的过程表明，没有任何药物残留超过韩国最大残留限量（MRL）。这种评估方法可以可靠地鉴定和定量渔业产品中的多类兽药，并且可以成为检查韩国目前禁止或不批准用于水产养殖的药物的有效手段。