摘要
本试验通过对仪器条件、前处理条件的优化,建立了牛羊肉组织中3种抗结核药物的UPLC-MS/MS多残留检测方法。样品通过提取,用QuEChERS法净化,C18柱(2.1 mm×100 mm,1.7μm)分离,0.2%甲酸水溶液和乙腈为流动相进行梯度洗脱,电喷雾离子化(ESI+)和多反应监测模式(MRM)检测,外标法定量。结果表明,在浓度为0.1~20.0μg/L范围内,利福平、利福喷汀和利福布汀呈良好线性,相关系数(r~2)大于0.99,利福平、利福喷丁和利福布汀的检出限和定量限分别为0.30、0.31、0.22μg/kg和1.02、1.03、0.73μg/kg。3种目标化合物利福平、利福喷丁、利福布汀在牛肉的平均回收率分别介于62.8%~109.2%、61.1%~115.4%、66.3%~105.9%之间,相对标准偏差(RSD,n=6)分别为4.0%~16.3%,4.3%~14.3%,4.6%~10.0%,方法的精密度与准确度满足相关标准的要求。3种目标化合物利福平、利福喷丁、利福布汀在羊肉的平均回收率分别介于62.1%~94.2%、61.6%~114.6%、61.2%~108.5%之间,相对标准偏差(RSD,n=6)分别为9.2%~15.8%,11.2%~18.9%,3.0%~11.3%,方法的精密度与准确度满足相关标准的要求。该方法具有灵敏、简单、高效的特点。
Aiming at anti-tuberculosis antibiotics in animal tissues,this study established the UPLC-MS/MS method for multi-residue detection of 3 anti-tuberculosis drugs in mutton and beef tissues by optimizing the pre-treatment conditions of instrument conditions.Samples were extracted by acidified acetonitrile ultrasonic and purified by HLB solid phase extraction column or QuEChERS,C18 The separation was performed on a column(2.1mm 100mm,1.7 m)with gradient elution of 0.2% formic acid aqueous solution and acetonitrile as mobile phases,and detected by electrospray ionization(ESI+)and multiple reaction monitoring mode(MRM).The results showed that rifampicentin and rifambutin showed good linearity in the range of 0.1 ~ 20.0 g/L,and the correlation coefficient(R~2)was greater than 0.99.The limits of detection and quantitation of rifampicentin and rifambutin were 0.30 0.31 0.22 g/kg and 1.02 1.03,respectively The average recoveries of rifampicin,rifapentine and rifambutin in beef were 62.8% ~ 109.2%,61.1% ~ 115.4%,66.3% ~ 105.9%,with relative standard deviations(RSD,n=6)of 4.0% ~ 16.3% and 4.3% ~ 14.3%,4.6% ~ 10.0%,respectively,the precision and accuracy of the method meet the requirements of relevant standards.The average recoveries of rifampicin,rifapentine and rifambutin in lamb were 62.1% ~ 94.2%,61.6% ~ 114.6%,61.2% ~ 108.5%,and the relative standard deviations(RSD,n=6)were 9.2% ~ 15.8%,11.2% ~ 18.9%,3.0% ~ 11.3%,the precision and accuracy of the method meet the requirements of relevant standards.The method has the characteristics of sensitivity,simplicity and efficiency.
作者
魏佩玲
胡波
张蓉银
陆向梅
宫平
WEI Peiling;HU Bo;ZHANG Rongyin;LU Xiangmei;GONG Ping(Institute of animal husbandry quality standards,Xinjiang Academy of animal husbandry Sciences,Urumqi,Xinjiang 830000,China)
出处
《中国饲料》
北大核心
2022年第14期69-72,共4页
China Feed
基金
新疆维吾尔自治区科技援疆计划项目(2018E02054)
新疆畜产品质量安全重点实验室(XJXS1412)。
关键词
牛羊肉
抗结核药物
多残留检测
beef and mutton
antituberculous drugs
multiple residue detection
