QuEChERS-超高效液相串联质谱测定淡水鱼中地西泮和奥沙西泮  

Determination of diazepam and oxazepam in freshwater fishes by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘虹[1] 曾远伟[1] 许惠雅 王咏欣 LIU Hong;ZENG Yuanwei;XU Huiya;WANG Yongxin(Guangzhou Yuexiu District Center for Disease Control and Prevention,Guangzhou,Guangdong 510055,China)

机构地区：[1]广州市越秀区疾病预防控制中心理化检验科,广东广州510055

出　　处：《职业与健康》2024年第21期2913-2918,2924,共7页Occupation and Health

基　　金：广州市卫生健康科技项目(20241A041001)。

摘　　要：目的水产品中药物残留现象日益严重,地西泮、奥沙西泮是淡水鱼中常用的镇静类药物,长期摄入将对人体产生极大危害。本研究建立并优化了淡水鱼中地西泮和奥沙西泮药物残留的QuEChERS-超高效液相色谱串联质谱测定方法。方法样品以乙腈作为提取剂,经超声提取,通过QuEChERS试剂(100 mg PSA,50 mg C_(18),150 mg MgSO_(4))净化,采用甲醇-0.1%甲酸水洗脱,色谱柱ACQUITY UPLC BEH C_(18)(50 mm×2.1 mm,1.7μm)分离,正离子扫描,电喷雾串联质谱多反应监测模式(multi reaction monitoring,MRM)检测,内标法定量。结果地西泮和奥沙西泮在0.05~50.00μg/L范围内线性关系良好(r>0.999),地西泮和奥沙西泮检出限和定量限分别为0.5和1.0μg/kg。以1、2和20倍检出限进行3个水平加标试验(n=6),地西泮和奥沙西泮回收率范围为81.1%~98.3%,相对标准偏差均小于10%。结论所研究的方法前处理净化方式方便快捷、步骤简单、重现性好,以0.1%甲酸水作为流动相大幅度提高待测物响应值,适用于淡水鱼中地西泮和奥沙西泮的定性定量分析。Objective The phenomenon of drug residues in aquatic products is becoming increasingly serious.Diazepam and oxazepam are commonly used sedative drugs in freshwater fish,and long-term consumption will cause great harm to the human body.This study established and optimized a QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(Qu EChERS-UPLC-MS)method for the determination of diazepam and oxazepam drug residues in freshwater fish.Methods The sample was extracted with acetonitrile,subjected to ultrasonic extraction,purified by QuEChERS method(100 mg PSA,50 mg C_(18),150 mg MgSO_(4)),and finally eluted with methanol-0.1% formic acid water,separated by chromatography column ACQUITY UPLC BEH C_(18)(50 mm×2.1 mm,1.7μm),scanned by positive ions,detected by electrospray tandem mass spectrometry multi reaction monitoring(MRM),and quantified by internal standard method.Results The linear relationship between diazepam and oxazepam was good within the range of 0.05-50.00μg/L(r>0.999).The limits of detection(LOD)and quantification(LOQ)of diazepam and oxazepam were 0.5 and 1.0μg/kg,respectively.The mean recoveries of diazepam and oxazepam ranged from 81.1% to 98.3% at the spiked levels of 1,2,and 20 times detection limits(n=6),with the relative standard deviations(RSD)less than 10%.Conclusion The pre-treatment process of this method is convenient,and fast,simple in steps,with good reproducibility.Using 0.1% formic acid water as the mobile phase significantly improves the response value of the tested substance.This method is suitable for the qualitative and quantitative analysis of diazepam and oxazepam in freshwater fishes.

关 键 词：地西泮 奥沙西泮 QUECHERS 超高效液相色谱-串联质谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]