超高效液相色谱串联质谱法同时测定渔用非药品类投入品中喹乙醇、氯霉素类、硝基呋喃类药物残留

Simultaneous determination of olaquindox,chloramphenicol and nitrofuran residues in fishery non-pharmaceutical inputs by ultra performance liquid chromatography tandem mass spectrometry

本实验旨在建立超高效液相色谱串联质谱(UHPLC-MS/MS)同时测定渔用非药品类投入品中喹乙醇、氯霉素类、硝基呋喃类共8种药物残留的检测方法。使用乙腈作为提取剂,在避光的环境中对投入品中的8种药物进行涡旋超声提取,使用固相萃取柱对提取液进行净化后仪器分析,液相色谱以水和乙腈作为流动,使用BEH C18色谱柱对药物进行分离,质谱使用正负离子切换模式进行同时扫描,喹乙醇和硝基呋喃类药物使用基质匹配标线外标法定量,氯霉素类药物以氘代氯霉素作为内标物使用基质匹配标线内标法定量。结果表明:喹乙醇和硝基呋喃类的线性范围为0.5~20.0 ng/mL,氯霉素类的线性范围为0.2~20.0 ng/mL,标准曲线的相关系数为0.9987~0.9996,8种药物的方法检测限为1.0~2.5μg/kg,定量限为2.5~5.0μg/kg。使用2种空白投入品进行3个浓度的加标实验,回收率为75.5%~102.2%,相对标准偏差为2.8%~10.2%。本方法可同时对8种药物进行提取测定,检测效率较高,同时方法的准确度和精密度较好,可以用于渔用非药品类投入品中8种药物残留的测定。

An ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)method was developed for the simultaneous determination of olaquindox,chloramphenicol and nitrofuran residues in fishery non-pharmaceutical inputs.Acetonitrile was used as the extraction agent,and eight drugs in the input were extracted by vortex ultrasound in a dark environment.The solid phase extraction column was used to purify the extract and analyze the instrument.The liquid chromatography was carried out with water and acetonitrile as the flow.The BEH C18 column was used to separate the drugs,and the mass spectrometry was scanned simultaneously in the positive and negative ion switching mode.The olaquindox and nitrofuran drugs were quantified by matrix-matched external standard method,and the chloramphenicol drugs were quantified by matrix-matched internal standard method with deuterated chloramphenicol as internal standard.The results showed that the linear range of olaquindox and nitrofurans was 0.5~20.0 ng/mL,and the linear range of chloramphenicol was 0.2~20.0 ng/mL.The correlation coefficient of the standard curve was 0.9987~0.9996.The limit of detection of the eight drugs was 1.0~2.5μg/kg,and the limit of quantitation was 2.5~5.0μg/kg.The recoveries were 75.5%~102.2%,and the relative standard deviations were 2.8%~10.2%.This method could be used to extract and determine 8 kinds of drugs at the same time.The detection efficiency was high,and the accuracy and precision of the method were good.It could be used for the determination of 8 drug residues in fishery non-pharmaceutical inputs.