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

中文关键词:  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

英文关键词:ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry  mixed feed additive  illegal addition

中文摘要:

      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, 1.7 μm)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2.0~100.0 μg/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。

英文摘要:

      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, 1.7 μm) 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?100.0 μg/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.