Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Federal de Defesa Agropecuária, Seção Laboratorial Avançada em Santa Catarina (SLAV/SC/LFDA/RS), São José, SC 88102-600, Brazil.
Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Federal de Defesa Agropecuária, Seção Laboratorial Avançada em Santa Catarina (SLAV/SC/LFDA/RS), São José, SC 88102-600, Brazil; Instituto Catarinense de Sanidade Agropecuária (ICASA), Florianópolis, SC 88034-100, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Sep 1;1152:122232. doi: 10.1016/j.jchromb.2020.122232. Epub 2020 Jun 10.
A fast and simple method for the determination of 62 veterinary drugs in feedingstuffs was developed, optimized, validated, and applied to real samples. Sample preparation was based on a pressurized liquid extraction method using a hard cap coffee machine, which was compared to a commercial pressurized liquid extraction system. Extraction was performed with diatomaceous earth, acetonitrile (20%), and formic acid (0.1%). A central composite design was used to optimize the composition of the extraction solvent. The extracts were analyzed using two chromatographic modes (reversed phase with C and HILIC). Analytical limits were set to 25 (limit of detection) and 75 µg kg (limit of quantitation). For banned substances, a salting-out step was included, achieving LOQ lower as 1 µg kg for ractopamine. Other figures of merit such as precision, trueness, decision limit (CC), method capability (CC), matrix effects, stability, recovery, and measurement uncertainty were also reported for analytical validation. The method was successfully applied to hundreds of real samples demonstrating its fitness-for-purpose for the analysis of sulfonamides, tetracyclines, fluoroquinolones, avermectins, quinolones, beta-agonists, beta-lactams, amphenicols, benzimidazoles, coccidiostats, lincosamides, macrolides, nitrofurans, quinoxalines, melamine, and trimethoprim.
建立、优化、验证并应用于实际样品的快速、简单的饲料中 62 种兽药检测方法。样品制备基于加压液体萃取法，使用硬壳咖啡机制备，与商用加压液体萃取系统进行了比较。萃取时使用硅藻土、乙腈（20%）和甲酸（0.1%）。采用中心复合设计优化萃取溶剂的组成。采用两种色谱模式（反相和 HILIC）分析提取物。分析限值设定为 25（检测限）和 75µgkg（定量限）。对于禁用物质，包括盐析步骤，使得莱克多巴胺的 LOQ 低至 1µgkg。还报告了其他评价指标，如精密度、准确度、决策限（CC）、方法能力（CC）、基质效应、稳定性、回收率和测量不确定度，以进行分析验证。该方法成功应用于数百个实际样品，证明其适用于磺胺类、四环素类、氟喹诺酮类、阿维菌素类、喹诺酮类、β-激动剂、β-内酰胺类、安普霉素类、苯并咪唑类、球虫抑制剂、林可酰胺类、大环内酯类、硝基呋喃类、喹喔啉类、三聚氰胺和甲氧苄啶的分析。
