Hajrulai-Musliu Zehra, Uzunov Risto, Jovanov Stefan, Jankuloski Dean, Stojkovski Velimir, Pendovski Lazo, Sasanya James Jacob
Faculty of Veterinary Medicine-Skopje, University "Ss. Cyril and Methodius", Lazar Pop-Trajkov 5/7, 1000, Skopje, Republic of North Macedonia.
International Atomic Energy Agency, Vienna International Centre, P. O. Box 100, 1400, Vienna, Austria.
BMC Chem. 2021 Dec 8;15(1):62. doi: 10.1186/s13065-021-00788-5.
A multi-class and multi-residue/contaminant method for the determination of veterinary drug and pesticide residues and mycotoxins in bovine meat has been developed and validated. The veterinary drug residues/contaminants included antimicrobials, anabolic hormones, lactones, β-agonists, mycotoxins, and pesticides. Isotopic labeled internal standards were included to compensate residual matrix effects. The calibrators used in the method demonstrated linearity with the R > 0.98. The decision limit (CCα) values were in the range from 0.067 to 2103.84 μg/kg, while the range for detection capability (CCβ) was from 0.083 to 2482.13 μg/kg. The limit of detection (LOD) and limit of quantification (LOQ) were in the range from 0.059 to 291.36 μg/kg, and 0.081 to 328.13 μg/kg, respectively. The recovery of analytes ranged from 61.28% to 116.20%. The intra-day coefficient of variation (CV) was from 0.97 to 25.93% and the inter-day CV was 2.30-34.04%. The method has been used for the determination of 49 residues/contaminants in bovine meat. Application of the method in routine analysis in bovine samples, revealed in limited samples the presences of enrofloxacin, oxytetracycline and sulfadiazine at the concentration of 35.22 µg/kg, 27.35 µg/kg, and 36.20 µg/kg, respectively.
已开发并验证了一种用于测定牛肉中兽药和农药残留以及霉菌毒素的多类别、多残留/污染物方法。兽药残留/污染物包括抗菌剂、同化激素、内酯、β-激动剂、霉菌毒素和农药。采用同位素标记内标来补偿残留基质效应。该方法中使用的校准物显示出线性关系,相关系数R>0.98。决策限(CCα)值范围为0.067至2103.84μg/kg,而检测能力(CCβ)范围为0.083至2482.13μg/kg。检测限(LOD)和定量限(LOQ)分别在0.059至291.36μg/kg以及0.081至328.13μg/kg范围内。分析物的回收率在61.28%至116.20%之间。日内变异系数(CV)为0.97%至25.93%,日间CV为2.30%至34.04%。该方法已用于测定牛肉中的49种残留/污染物。该方法在牛样品常规分析中的应用显示,在有限的样品中分别检测到恩诺沙星、土霉素和磺胺嘧啶,浓度分别为35.22μg/kg、27.35μg/kg和36.20μg/kg。