Detection of Tetracycline Residue in Livestock and Poultry Wastewater by SPE-HPLC——Optimization Of Multi-media Detection Based on Plant Purification System
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.
tetracyclinelivestock and poultry wastewatersolid-phase extraction(SPE)high performance liquid chromatography(HPLC)