分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
10期
1478-1485
,共8页
李晴%罗辉泰%黄晓兰%朱志鑫%吴惠勤
李晴%囉輝泰%黃曉蘭%硃誌鑫%吳惠勤
리청%라휘태%황효란%주지흠%오혜근
四级杆飞行时间串联质谱%四环素类%磺胺类%喹诺酮类%三苯甲烷类%雄激素%孕激素%糖皮质激素%高通量%药物筛查
四級桿飛行時間串聯質譜%四環素類%磺胺類%喹諾酮類%三苯甲烷類%雄激素%孕激素%糖皮質激素%高通量%藥物篩查
사급간비행시간천련질보%사배소류%광알류%규낙동류%삼분갑완류%웅격소%잉격소%당피질격소%고통량%약물사사
Quadrupole-time-of-flight mass spectrometry%Tetracycliens%Sulfonamides%Quinolones%Triphenylmethanes%Estrogens%Androgens%Glucocorticoids%High throughput screening
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。
建立瞭以QuEChERS樣品預處理方法、四級桿飛行時間串聯質譜( Q-TOF MS)為檢測手段,針對魚肉中的四環素類、磺胺類、喹諾酮類、三苯甲烷類、雄激素、孕激素和糖皮質激素7類59種殘留藥物的快速篩查技術。通過正交實驗得到優化條件為:Na2 EDTA-Mcllvaine為緩遲溶液,乙腈為提取劑,淨化劑無水MgSO4、十八烷基鍵閤硅膠(C18)和N-丙基乙二胺(PSA)的用量分彆為每毫升提取液加入25,12.5和6.25 mg。對Q-TOF質譜篩查齣的暘性樣品,再用LC-MS/MS對樣品進行確證。本方法對59種藥物的檢齣下限為0.5~5.3μg/kg。本方法快速、簡單、可靠,可篩查的漁藥種類覆蓋麵廣,靈敏度滿足水產品藥物殘留檢測的要求,適用于魚類水產品中殘留藥物的快速測定。
건립료이QuEChERS양품예처리방법、사급간비행시간천련질보( Q-TOF MS)위검측수단,침대어육중적사배소류、광알류、규낙동류、삼분갑완류、웅격소、잉격소화당피질격소7류59충잔류약물적쾌속사사기술。통과정교실험득도우화조건위:Na2 EDTA-Mcllvaine위완충용액,을정위제취제,정화제무수MgSO4、십팔완기건합규효(C18)화N-병기을이알(PSA)적용량분별위매호승제취액가입25,12.5화6.25 mg。대Q-TOF질보사사출적양성양품,재용LC-MS/MS대양품진행학증。본방법대59충약물적검출하한위0.5~5.3μg/kg。본방법쾌속、간단、가고,가사사적어약충류복개면엄,령민도만족수산품약물잔류검측적요구,괄용우어류수산품중잔류약물적쾌속측정。
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 ) , 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.