摘要
建立了以QuEChERS样品预处理方法、四级杆飞行时间串联质谱（ Q-TOF MS）为检测手段,针对鱼肉中的四环素类、磺胺类、喹诺酮类、三苯甲烷类、雄激素、孕激素和糖皮质激素7类59种残留药物的快速筛查技术。通过正交实验得到优化条件为：Na2 EDTA-Mcllvaine为缓冲溶液,乙腈为提取剂,净化剂无水MgSO4、十八烷基键合硅胶（C18）和N-丙基乙二胺（PSA）的用量分别为每毫升提取液加入25,12.5和6.25 mg。对Q-TOF质谱筛查出的阳性样品,再用LC-MS/MS对样品进行确证。本方法对59种药物的检出下限为0.5～5.3μg/kg。本方法快速、简单、可靠,可筛查的渔药种类覆盖面广,灵敏度满足水产品药物残留检测的要求,适用于鱼类水产品中残留药物的快速测定。
A high-throughput method for screening drug multi residues was developed by quadrupole-time-of-flight（ Q-TOF） mass spectrometry together with QuEChERS sample preparation technique. It has been used for the determination of 57 drugs, such as tetracyclines （ TCs ） , sulfonamides （ SAs ） , quinolones （ QNs ） ,＆amp;nbsp;triphenylmethanes （TPMs）, estrogens （ETs）, androgens （AGs） and glucocorticoids （GCs） in fish. The optimized pretreatment conditions were examined. The target compounds were extracted with acetonitrile under the condition of Na2 EDTA-Mcllvaine buffer, and the usage of clean-up reagents was 25 mg anhydrous magnesium sulfate, 12. 5 mg octadecylsilane and 6. 25 mg N-Propylethylenediamine sorbent for extracted solvent of each milliliter. The positive results acquired by this high-throughput method were confirmed by liquid chromatography-tandem mass spectrometry （ LC-MS/MS） . The detection limit for these 59 drugs was in the range of 0. 5-5. 3 μg/kg. The method is time-saving, convenient, effective and wide coverage. Its sensitivity can meet the requirement of the detection of drug residues in aquatic products.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第10期1478-1485,共8页
Chinese Journal of Analytical Chemistry
基金
广东省科技厅科技计划重点项目(No.2012A020100002)资助
