QuEChERS技术结合高效液相色谱-串联质谱法测定鱼肉中6种替考拉宁残留量  

Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with QuEChERS Method

作　　者：金慧 赵城[2] 郑光明 魏琳婷[2] 史晓娜 林嘉薇 李丽春 单奇[2] 马丽莎[2] 尹怡[1,2] JIN Hui;ZHAO Cheng;ZHENG Guang-ming;WEI Lin-ting;SHI Xiao-na;LIN Jia-wei;LI Li-chun;SHAN Qi;MA Li-sha;YIN Yi(College of Food Science and Technology,Shanghai Ocean University,Shanghai 201306,China;Pearl River Fisheries Research Institute,Chinese Academy of Fishery Sciences/Laboratory of Aquatic Product Quality and Safety Risk Assessment,Ministry of Agriculture and Rural Affairs(Guangzhou)/Key Laboratory of Aquatic Animal Immune Technology of Guangdong Province,Guangzhou 510380,China)

机构地区：[1]上海海洋大学食品学院,上海201306 [2]中国水产科学研究院珠江水产研究所/农业农村部水产品质量安全风险评估实验室(广州)/广东省水产动物免疫技术重点实验室,广东广州510380

出　　处：《分析测试学报》2022年第6期835-842,共8页Journal of Instrumental Analysis

基　　金：中国-东盟海上合作基金项目(CAMC-2018F)。

摘　　要：采用QuEChERS前处理技术,建立了鱼肉中6种替考拉宁组分的高效液相色谱-串联质谱检测方法。搅碎均匀的鱼肉样品经乙腈-10%三氯乙酸(6∶4,体积比)提取,100 mg乙二胺-N-丙基硅烷(PSA)净化后,使用Agilent SB C_(18)(2.1 mm×100 mm,1.8μm)色谱柱分离,以0.1%甲酸乙腈和0.1%甲酸为流动相进行梯度洗脱,采用电喷雾电离正离子(ESI+),多反应监测模式(MRM)进行检测,内标法定量。考察了提取溶剂种类与体积、吸附剂种类与用量对目标化合物回收率的影响。评价了6种目标物在不同鱼肉基质中的基质效应。在优化条件下,6种替考拉宁组分在4 min内得到良好分离。目标物在各自浓度范围内线性良好,相关系数(r2)均不小于0.998;在5.0、10.0、25.0μg/kg 3个加标水平下,各组分的回收率为84.3%~93.3%,日内相对标准偏差和日间相对标准偏差(n=6)分别不大于7.0%和6.2%,方法的检出限和定量下限分别为0.5~2.0μg/kg和2.0~5.0μg/kg。采用该方法对采集的9种40个鱼肉样品进行检测,所有样品均未检出替考拉宁组分。该方法简单、灵敏、准确、可靠,可用于鱼肉中6种替考拉宁组分的定量分析。A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)with QuEChERS pretreatment was developed for the simultaneous determination of six teicoplanins in fish samples.The six components in minced fish samples were extracted with acetonitrile-10%trichloroacetic acid(6∶4)mixed solution.Then the extracted supernatant was cleaned up with 100 mg of primary secondary amine(PSA).Separation of the targets was performed on an Agilent SB C_(18) chromatographic column(2.1 mm×100 mm,1.8μm)by gradient elution,using 0.1%formic acetonitrile and 0.1%formic as the mobile phase A and the mobile phase B,respectively.The six targets were detected in positive ion electrospray ionization mode(ESI+)under multiple reaction monitoring(MRM)mode,then quantified by the internal standard method with polymyxin sulfate B as the internal standard(IS).Effects of different types and volumes of extraction solvent,different types and dosages of adsorbent on recoveries of six targets were investigated in detail.The matrix effects of six teicoplanins in different fish substrates were evaluated by the ratio of solvent standard curve and matrix-matched standard curve.Under the optimal conditions,six teicoplanins were well separated by HPLC-MS/MS within 4 min.Good linear relationships were obtained for six analytes in the concentration range of 1-100μg/L,with their correlation coefficients(r2)greater than 0.998.At three spiked levels of 5.0,10.0 and 25.0μg/kg,the average recoveries for six analytes in different fish samples ranged from 84.3%to 93.3%,with intra-day relative standard deviations(intra-RSDs)and inter-day relative standard deviations(inter-RSDs)not more than 7.0%and 6.2%,respectively.The limits of detection(LODs)and limits of quantitation(LOQs)were in the range of 0.5-2.0μg/kg and 2.0-5.0μg/kg,respectively.The established method was applied to the detection of teicoplanins in various fish samples(forty fish samples that were divided into nine varieties,containing carp,crucian,grass carp,chub,silver carp,mandarin

关 键 词：替考拉宁 QuEChERS技术 高效液相色谱-串联质谱(HPLC-MS/MS) 鱼肉 

分 类 号：O657.63[理学—分析化学] O629.5[理学—化学]