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
佘婷婷 1彭诗怡 1余乐洹 1熊学玲 1王森 1余美泽 1邓雅亭 1叶桂梅1
作者信息
- 1. 广东第二师范学院 生物与食品工程学院,广东 广州 510303
- 折叠
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Na2EDTA-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Na2EDTA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3.83 μg/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～655.94 μg/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.
Abstract
By optimizing the pretreatment conditions,a solid-phase extraction(SPE)high performance liquid chro-matography(HPLC)methodological sequence for detecting tetracycline residues in different types of sample ma-trix was established.Sediment and plant tissue samples were extracted with Na2 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 3.83 μg/L,0.15 mg/kg,and 1.53 mg/kg,respective-ly.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 sys-tem,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Key words
tetracycline/livestock and poultry wastewater/solid-phase extraction(SPE)/high performance liquid chromatography(HPLC)引用本文复制引用
出版年
2024
NETL
NSTL
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