摘要
目的建立超高效液相色谱-四极杆飞行时间质谱法快速测定混合型饲料添加剂中培氟沙星、氯霉素、沙丁胺醇、盐酸克伦特罗、氧氟沙星、恩诺沙星、诺氟沙星、氟苯尼考、磺胺嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、甲硝唑、多西环素、金刚烷胺共14种化学药物的分析方法。方法样品经乙腈-水(8:2,V:V)提取,上清液离心后上样,以0.1%(V:V)甲酸甲醇溶液和0.1%(V:V)甲酸水溶液为流动相进行梯度洗脱(负离子模式流动相为乙腈-水),C18色谱柱(50 mm×2.1 mm,1.7μm)分离。分别采用正/负离子模式检测分析。结果14种药物的质量数误差绝对值小于5 mDa,在2.0~100.0μg/L范围内线性关系良好,相关系数大于0.99。4个浓度水平的平均回收率为70.6%~119.80%,相对标准偏差1.0%~12.4%。结论该方法操作简便、结果准确,适用于混合型饲料添加剂中非法添加药物的快速筛查分析。
Objective To establish a method for the rapid determination of 14 kinds of chemical drugs including pefloxacin,chloramphenicol,salbutamol,clenbuterol hydrochloride,ofloxacin,enrofloxacin,norfloxacin,florfenicol,sulfadiazine,sulfamethoxazole,sulfamonomethoxine,metronidazole,doxycycline and amantadine in a mixed type feed additive by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry.Methods The samples(8:2,V:V)were extracted by acetonitrile-water.The supernatant was centrifuged and loaded into a C18 column(50 mm×2.1 mm,1.7μm)with gradient elution using 0.1%(V:V)formic acid in methanol and 0.1%(V:V)formic acid in water as the mobile phases.Positive/negative ion mode detection analysis was adopted respectively.Results The absolute values of mass error of the 14 drugs were less than 5 mDa,and the linear relationship was good within the range of 2.0-100.0μg/L,with the correlation coefficient greater than 0.99.The average recoveries at 4 concentration levels were 70.6%-119.80%,and the relative standard deviations were 1.0%-12.4%.Conclusion This method is simple and accurate,and is suitable for rapid screening and analysis of illegally added drugs in mixed feed additives.
作者
吴蕾
吴昊
张莉
许世富
刘红云
蔡一杰
许晓靖
WU Lei;WU Hao;ZHANG Li;XU Shi-Fu;LIU Hong-Yun;CAI Yi-Jie;XU Xiao-Jing(Anhui Institute of Veterinary Drug and Feed Inspection,Hefei 230091,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第8期3104-3112,共9页
Journal of Food Safety and Quality
关键词
超高效液相色谱串联飞行时间质谱法
混合型饲料添加剂
非法添加
ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry
mixed feed additive
illegal addition
