Key Lab of New Animal Drug of Gansu Province, Key Lab of Veterinary Pharmaceutical Development of Ministry of Agriculture and Rural Affairs, Lanzhou Institute of Husbandry and Pharmaceutical Sciences of CAAS, Lanzhou 730050, China.
Key Laboratory of Pesticides and Veterinary Drugs Monitoring for State Market Regulation, Lanzhou Institute for Food and Drug Control, Lanzhou 730050, China.
Molecules. 2024 Sep 27;29(19):4599. doi: 10.3390/molecules29194599.
Rifaximin and rifampicin are good broad-spectrum antimicrobials. The irrational use of antimicrobial drugs in veterinary clinics could threaten public health and food safety. It is necessary to develop a reliable detection method of the residue for enhancing the rational supervision of the use of such drugs, reducing and slowing down the generation of bacterial resistance, and promoting animal food safety and human health. So, this study developed an LC-MS/MS method for the detection of rifaximin and rifampicin residues in animal-origin foods. The residual rifaximin and rifampicin of homogenized test materials were extracted with acetonitrile-dichloromethane solution or acetonitrile in the presence of anhydrous sodium sulfate and vitamin C, purified by dispersible solid phase extraction, determined by LC-MS/MS, and quantified by the internal standard method. The specificity, sensitivity, matrix effect, accuracy, and precision of the method were investigated in the edible tissues of cattle, swine, or chicken. In addition, the stability of the standard stock solution and the standard working solution was also investigated. The method was suitable for the muscle, liver, kidney, fat, milk, and eggs of cattle, swine, or chicken, as well as fish and shrimp. The specificity of the method was good, and the detection of the analytes was not affected by different matrices. Both the LOD and LOQ of the two analytes were 5 μg/kg and 10 μg/kg, respectively. The results of matrix effects in each tissue were in the range of 80-120%; there were no significant matrix effects. The average accuracy of rifaximin and rifampicin in different foodstuffs of animal origin was between 80% and 120%, and the method precision was below 20% (RSD). The proposed method showed good performance for determination, which could be employed for the extraction, purification, and detection of residual rifaximin and rifampicin in edible animal tissues. The pretreatment procedure of tissue samples was simple and feasible. The method was highly specific, stable, reliable, and with high sensitivity, accuracy, and precision, which met the requirements of quantitative detection of veterinary drug residues.
利福昔明和利福平是广谱抗菌药物。兽医临床抗菌药物的不合理使用可能会威胁到公共卫生和食品安全。因此,有必要开发一种可靠的残留检测方法,以加强此类药物使用的合理监管,减少和减缓细菌耐药性的产生,促进动物食品安全和人类健康。因此,本研究建立了一种用于检测动物源食品中利福昔明和利福平残留的 LC-MS/MS 方法。在无水硫酸钠和维生素 C 的存在下,用乙腈-二氯甲烷溶液或乙腈提取均质测试材料中的残留利福昔明和利福平,用分散固相萃取法净化,用 LC-MS/MS 测定,并用内标法定量。在牛、猪或鸡的食用组织中考察了方法的特异性、灵敏度、基质效应、准确度和精密度。此外,还考察了标准储备溶液和标准工作溶液的稳定性。该方法适用于牛、猪或鸡的肌肉、肝脏、肾脏、脂肪、牛奶和鸡蛋,以及鱼类和虾类。该方法的特异性良好,不同基质对分析物的检测没有影响。两种分析物的 LOD 和 LOQ 均为 5μg/kg 和 10μg/kg。各组织中基质效应的结果均在 80-120%范围内;不存在显著的基质效应。利福昔明和利福平在动物源性不同食品中的平均准确度在 80%-120%之间,方法精密度均低于 20%(RSD)。该方法在检测方面表现出良好的性能,可用于食用动物组织中残留利福昔明和利福平的提取、净化和检测。组织样品的预处理程序简单可行。该方法具有高度的特异性、稳定性、可靠性和高灵敏度、准确度和精密度,满足兽药残留定量检测的要求。