高效液相色谱-三重四极杆复合线性离子阱质谱法检测水产品中氟喹诺酮类抗生素和镇静剂  

Detection of Fluroquinolone Antibiotics and Sedatives in Aquatic Products by High Performance Liquid Chromatography-Triple Quadrupole/Composite Linear Ion Trap Mass Spectrometry

作　　者：穆树荷 封腾望 刘欢[2,3] 孙慧武 李晋成[2,3] MU Shuhe;FENG Tengwang;LIU Huan;SUN Huiwu;LI Jincheng(College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306,China;Chinese Academy of Fishery Sciences,Beijing100141,China;Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture and Rural Affairs,Beijing100141,China)

机构地区：[1]上海海洋大学水产与生命技术学院,上海201306 [2]中国水产科学研究院,北京100141 [3]农业农村部水产品质量安全控制重点实验室,北京100141

出　　处：《理化检验（化学分册）》2023年第5期561-568,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：中央级公益性科研院所基本科研业务项目(2020B005);中国水产科学研究院科技创新项目(2020TD75)。

摘　　要：为实现水产品中抗生素和镇静剂的同时、快速检测,进行了题示研究。分取2.0 g匀浆后的样品的肌肉组织,加入体积比79∶1∶20的乙腈-乙酸-水混合溶液10 mL,振荡1 min,超声10 min。加入2.0 g氯化钠,振荡1 min,于-20℃保存30 min,用于去除提取液中的脂肪。离心10 min,分取1 mL上清液注入装载有150 mg C18的CAFS clean-up净化柱中,多次推动活塞,将提取液全部转移到2 mL离心管中。分取0.5 mL净化液,加入0.5 mL 0.1%(体积分数,下同)甲酸溶液,混匀后过0.22μm尼龙滤膜。滤液注入高效液相色谱-三重四极杆复合线性离子阱质谱仪,9种目标物在BEH C18色谱柱上用不同体积比的0.1%甲酸溶液和含0.1%甲酸的甲醇溶液的混合溶液进行梯度洗脱分离后,用电喷雾离子源正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质匹配法定量。结果显示,9种目标物的质量分数分别在1.0~50.0μg·kg^(-1)(丁卡因、布比卡因、恩诺沙星和氧氟沙星)、2.0~50.0μg·kg^(-1)(地西泮和氟罗沙星)、5.0~50.0μg·kg^(-1)(环丙沙星、培氟沙星和洛美沙星)内与对应的峰面积呈线性关系,检出限为0.2~1.0μg·kg^(-1);对空白草鱼样品进行3个浓度水平的加标回收试验,回收率为99.1%~110%,测定值的相对标准偏差(n=6)分别为1.9%~8.2%(日内精密度试验)和2.6%~8.5%(日间精密度试验)。方法用于28份水产品的分析,检出了1种镇静剂布比卡因(检出量为1.41μg·kg^(-1))以及4种氟喹诺酮类抗生素[洛美沙星、培氟沙星、环丙沙星(3种抗生素检出量均低于测定下限)和恩诺沙星(检出量为2.43~4.61μg·kg^(-1),低于GB 31650-2019规定的限量)]。In order to realize the simultaneous and rapid determination of antibiotics and sedatives in aquatic products,the study mentioned by title was carried out.An aliquot(2.0g)of muscle tissue of the sample homogenized was taken,and 10mL of acetonitrile-acetic acid-water mixed solution at volume ratio of 79∶1∶20 was added.The mixture was shaken for 1min,ultrasonicated for 10min,and mixed with 2.0g of sodium chloride.The mixture was shaken for 1min,stored at-20℃for 30min to remove fat from the extract,and centrifuged for 10min.An aliquot(1mL)of supernatant was introduced into the CAFS clean-up column loaded with 150mg C18,and the extract was transferred into a 2mL-centrifuge tube by pushing the piston several times.An aliquot(0.5mL)of the purified solution was taken,and mixed with 0.5mL of 0.1%(volume fraction,the same below)formic acid solution.The mixed solution was passed through a 0.22μm nylon filter membrane,and the filtrate was introduced into the high performance liquid chromatograph-triple quadrupole/composite linear ion trap mass spectrometer,and the 9targets were separated on the BEH C18column with mixed solutions composed of 0.1%formic acid solution and methanol solution containing 0.1%formic acid at different volume ratios by gradient elution,ionized by ESI+mode,detected by MRM mode,and quantified by the matrix matching method.As shown by the results,linear relationships between values of the mass fraction and the peak area of the 9targets were kept in the ranges of 1.0-50.0μg·kg^(-1)(tetracaine,bupivacaine,enrofloxacin and ofloxacin),2.0-50.0μg·kg^(-1)(diazepam and fluroxacin),and 5.0-50.0μg·kg^(-1)(ciprofloxacin,pefloxacin and lomefloxacin),with detection limits(3S/N)in the range of 0.2-1.0μg·kg^(-1).Test for the spiked recovery was made on the blank grass carp sample in the 3 concentration levels,giving recoveries in the range of 99.1%-110%,and RSDs(n=6)of the determined values were in the ranges of 1.9%-8.2%(intra-day precision test)and 2.6%-8.5%(inter-day precision test).The proposed met

关 键 词：滤过型净化柱 高效液相色谱-三重四极杆复合线性离子阱质谱法 氟喹诺酮类抗生素 镇静剂 水产品 

分 类 号：O657.63[理学—分析化学]