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14种化学药物  

Rapid determination of 14 kinds of chemical drugs in mixed feed additives by ultra performance liquid chromatography-quadrupole time of flight mass spectrometry

作　　者：吴蕾[1] 吴昊[1] 张莉[1] 许世富[1] 刘红云[1] 蔡一杰[1] 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)

机构地区：[1]安徽省兽药饲料监察所,合肥230091

出　　处：《食品安全质量检测学报》2021年第8期3104-3112,共9页Journal of Food Safety and Quality

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.

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 

分 类 号：O657.63[理学—分析化学] S816.17[理学—化学]