盐析辅助液液萃取/高效液相色谱-串联质谱法测定渔业水体中的7种喹诺酮类抗生素  

Determination of Seven Quinolones Antibiotics in Fishery Water Using Salting-out Assisted Liquid-Liquid Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：杨霄[1,2] 刘伶俐 李小玲[1,2] 肖维 陈湘艺[1,2] 谢仲桂 YANG Xiao;LIU Ling-li;LI Xiao-ling;XIAO Wei;CHEN Xiang-yi;XIE Zhong-gui(Hunan Fisheries Science Institute,Changsha 410153,China;Fishery Products Quality Supervision and Testing Center,Ministry of Agriculture and Rural Affairs,Changsha 410153,China)

机构地区：[1]湖南省水产科学研究所,湖南长沙410153 [2]农业农村部渔业产品质量监督检验测试中心(长沙),湖南长沙410153

出　　处：《分析测试学报》2021年第10期1509-1514,共6页Journal of Instrumental Analysis

基　　金：湖南省科技重大专项(2017NK1030)。

摘　　要：利用盐析辅助液液萃取(SALLE)/高效液相色谱-串联质谱(HPLC-MS/MS)建立了测定渔业水体中环丙沙星等7种喹诺酮类抗生素的分析方法。水样用乙腈提取,硫酸镁盐析分层,提取液经氮吹浓缩后,采用Waters Atlantis C_(18)色谱柱(150 mm×2.1 mm,3.0μm)以0.1%(体积分数)甲酸水溶液-甲醇为流动相进行梯度洗脱,采用电喷雾正离子模式检测,外标法定量。实验考察了水样pH值、萃取剂、盐析剂以及涡旋混合时间对萃取效率的影响。在最优的实验条件下,7种喹诺酮类抗生素在各自的质量浓度范围内线性良好,相关系数(r^(2))均大于0.995,检出限(LOD)和定量下限(LOQ)分别为3~10 ng/L和10~25 ng/L。对空白水样进行3个水平的加标回收实验,回收率为77.8%~104%,相对标准偏差(RSD)为3.1%~10%。该方法简单、灵敏、高效,可应用于渔业水体中喹诺酮类抗生素的检测。A method for determination of seven quinolones antibiotics in fishery water was established based on salting-out assisted liquid-liquid extraction(SALLE)coupled with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Water samples were extracted with acetonitrile and layered with salting-out agent of magnesium sulfate.The acetonitrile solution was con⁃centrated under a stream of nitrogen gas.All antibiotics were separated by gradient elution on a Waters Atlantis C_(18) column(150 mm×2.1 mm,3.0μm)with the mobile phases of 0.1%(by volume)formic acid aqueous solution and methanol,and then analyzed with an electrospray ionization source in the positive ion mode.The external standard method was used for quantitative analysis of the antibiotics.Various parameters affecting the extraction process such as pH value of the water sample,type and vol⁃ume of extraction solvent,type and weight of salting-out agent and vortex agitation time were investigat⁃ed.Under the optimal conditions,the correlation coefficients(r^(2))of linear calibration curves were over 0.995 in the corresponding concentration ranges.The limits of detection(LOD)and the limits of quan⁃titation(LOQ)of the method were in the range of 3-10 ng/L and 10-25 ng/L,respectively.Recover⁃ies for the seven quinolones at three spiked levels ranged from 77.8%to 104%,with relative standard deviations(RSD)of 3.1%-10%.The method is simple,sensitive and effective,and could be used for the determination of seven quinolones antibiotics in fishery water.

关 键 词：盐析辅助液液萃取 高效液相色谱-串联质谱 喹诺酮类抗生素 渔业水体 

分 类 号：O657.7[理学—分析化学] S931.3[理学—化学]