Towards high throughput analysis using 96-well plate solid phase extraction to determine sedatives and β-blocker residues in food control monitoring

IF 5.7 2区化学 Q1 CHEMISTRY, ANALYTICAL Analytica Chimica Acta Pub Date : 2024-10-14 DOI:10.1016/j.aca.2024.343335

Ane Arrizabalaga-Larrañaga, Dieke van Doorn, Saskia S. Sterk

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Abstract

Background

Veterinary drugs are widely used in animal production to prevent infections and treat diseases but, this may cause a risk to consumers. Due to the high number of food samples required to monitor yearly, simple, fast, sensitive and selective analytical methods are needed in control laboratories to ensure consumers safety. Nevertheless, many analytical methodologies available in these laboratories include multiple steps and therefore are time-consuming and hinder the analysis throughput requiring significant amounts of solvents and reagents.

Results

This work developed a 96-well plate solid phase extraction (SPE) method for the extraction of seven sedatives and a β-blocker in animal kidney by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC−MS/MS). The developed method was validated based on Implementing Regulation (EU) 2021/808 in kidney, meat and fish. The performance characteristics of the validation (1–5 μg kg⁻¹) showed good linearity (R² > 0.998) while decision limits (CCα) were between 1 and 1.2 μg kg⁻¹. Trueness and precision were determined at three levels (n = 7) and the results showed values ranging from 85 to 103 % and from 1 to 9 %, respectively. The feasibility of the method was demonstrated for the residue control requirement established by EU. Method was applied to 201 samples of kidney, meat and fish.

Significance

This study is the first to present an optimized and validated holistic method for sedatives and β-blocker using 96-well plate SPE and UHPLC−MS/MS. The method showed good performance in kidney, meat and fish samples being an universal method for any species along the same type of sample. The fast, easy, efficient, reliable and universal method showed high throughput and so reduced the analysis time by nine-fold and the required solvent amount by four times fulfilling the green chemistry principals.

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利用 96 孔板固相萃取技术进行高通量分析，以确定食品控制监测中的镇静剂和 β-受体阻滞剂残留量

背景兽药被广泛用于动物生产中，以预防感染和治疗疾病，但这可能会给消费者带来风险。由于每年需要监测大量的食品样品，因此控制实验室需要简单、快速、灵敏和选择性强的分析方法来确保消费者的安全。然而，这些实验室现有的许多分析方法都包括多个步骤，因此耗时长，而且需要大量的溶剂和试剂，妨碍了分析的通量。结果这项工作开发了一种 96 孔板固相萃取 (SPE) 方法，利用超高效液相色谱-串联质谱 (UHPLC-MS/MS) 技术提取动物肾脏中的七种镇静剂和一种β-受体阻滞剂。根据实施条例（EU）2021/808，对所开发的方法在肾脏、肉类和鱼类中进行了验证。验证结果表明，该方法（1-5 μg kg-1）线性关系良好（R2 > 0.998），判定限（CCα）在 1 至 1.2 μg kg-1 之间。在三个水平（n=7）上测定了准确度和精密度，结果显示准确度和精密度分别为 85%至 103%和 1%至 9%。结果表明，该方法适用于欧盟规定的残留控制要求。本研究首次采用96孔板SPE和UHPLC-MS/MS对镇静剂和β-受体阻滞剂进行了整体优化和验证。该方法在肾脏、肉类和鱼类样品中表现出良好的性能，是一种适用于任何物种同类样品的通用方法。这种快速、简便、高效、可靠和通用的方法具有高通量，因此分析时间缩短了九倍，所需溶剂用量减少了四倍，符合绿色化学原则。

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来源期刊

Analytica Chimica Acta 化学-分析化学

CiteScore

10.40

自引率

6.50%

发文量

1081

审稿时长

38 days

期刊介绍： Analytica Chimica Acta has an open access mirror journal Analytica Chimica Acta: X, sharing the same aims and scope, editorial team, submission system and rigorous peer review. Analytica Chimica Acta provides a forum for the rapid publication of original research, and critical, comprehensive reviews dealing with all aspects of fundamental and applied modern analytical chemistry. The journal welcomes the submission of research papers which report studies concerning the development of new and significant analytical methodologies. In determining the suitability of submitted articles for publication, particular scrutiny will be placed on the degree of novelty and impact of the research and the extent to which it adds to the existing body of knowledge in analytical chemistry.