SPE-HPLC法检测畜禽养殖废水中四环素残留——基于植物净化系统多介质检测优化  

Detection of Tetracycline Residue in Livestock and Poultry Wastewater by SPE-HPLC-Optimization Of Multi-media Detection Based on Plant Purification System

作　　者：佘婷婷 彭诗怡 余乐洹 熊学玲 王森 余美泽 邓雅亭 叶桂梅 She Tingting;Peng Shiyi;Yu Lehuan;Xiong Xueling;Wang Sen;Yu Meize;Deng Yating;Ye Guimei(School of Biology and Food Engineering,Guangdong University of Education,Guangzhou 510303,Guangdong,China)

机构地区：[1]广东第二师范学院生物与食品工程学院,广东广州510303

出　　处：《绿色科技》2024年第12期107-111,共5页Journal of Green Science and Technology

基　　金：广东省普通高校重点领域专项(编号:2021ZDZX4004);广东第二师范学院大学生创新创业训练计划项目(编号:S202314278038);广东第二师范学院生态学科研团队项目(编号:广东二师〔2020〕58号)。

摘　　要：通过对前处理条件进行优化,建立了一套固相萃取(SPE)-高效液相色谱(HPLC)检测多介质中四环素残留量的方法。底泥和植物组织经Na_(2)EDTA-Mcllvaine的甲醇溶液(1∶1,v∶v,pH=4)提取后,分别以HLB小柱(底泥)和SAX/PSA-HLB串联柱(植物组织)富集净化;水样经Na_(2)EDTA溶液(pH=3.4)提取后,以HLB小柱富集净化后再进行HPLC检测。四环素添加浓度为5 mg/L(低浓度)和50 mg/L(高浓度)时,水体、底泥以及植物根系等3种基质中的加标回收率分别达到106.5±1.0%、90.7±8.0%、92.8±1.0%(5 mg/L)和93.9±1.8%、78.5±0.4%、78.8±0.4%(50 mg/L),方法准确度和精密度均较高。四环素在水体、底泥以及植物根系中的检出限分别为3.83μg/L、0.15 mg/kg以及1.53 mg/kg,方法在0~50 mg/L范围内具有良好的定量线性关系。应用该方法检测人工模拟畜禽养殖废水系统各介质样品,检出四环素浓度为nd~655.94μg/L(水体)和0.59~78.45 mg/kg(底泥、植物组织),表明该方法有效可行。By optimizing the pretreatment conditions,a solid-phase extraction(SPE)high performance liquid chromatography(HPLC)methodological sequence for detecting tetracycline residues in different types of sample matrix was established.Sediment and plant tissue samples were extracted with Na_(2)EDTA-McIlvaine solution in methanol(v∶v=1∶1,pH=4),and subsequently purified by HLB SPE column(sediment)or SAX/PSA-HLB tandem SPE columns(plant tissues).Water samples were extracted and purified by HLB SPE columns under pH=3.4,followed by HPLC detection.The recoveries of tetracycline in water,sediment,and plant roots were 106.5±1.0%,90.7±8.0%,92.8±1.0%at low spiking level of 5 mg/L,and 93.9±1.8%,78.5±0.4%,78.8±0.4%at high spiking level of 50 mg/L,respectively,indicating high accuracy and precision of the method.The method detection limits of tetracycline in water,sediment,and plant tissues were 3.83μg/L,0.15 mg/kg,and 1.53 mg/kg,respectively.Good linearity for calibration curve was showed within the range of 0~50 mg/L.The method was applied to determine tetracycline in various sample matrix from an artificial livestock and poultry wastewater treatment system,with detected concentrations ranging from nd~655.94 ng/L(water)and 0.59~78.45 mg/kg(sediment and plant tissues),demonstrating that the method is effective and feasible for field samples analysis.

关 键 词：四环素 畜禽养殖废水-植物净化系统 固相萃取 高效液相色谱法 

分 类 号：S52[农业科学—作物学]