固相萃取-高效液相色谱同时测定沼液中3种四环素类和6种磺胺类抗生素

建立了一种用固相萃取高效液相色谱法同时测定沼液中3种四环素类(TCs)和6种磺胺类(SAs)抗生素的分析方法.样品经Na2 EDTA提取,固相萃取小柱富集净化,甲醇洗脱后,用高效液相色谱-紫外检测法测定.检测波长270 nm,柱温25℃,流动相为乙腈-o.1％甲酸水溶液,采用等度洗脱.9种待测组分实现了基线分离,线性范围为0.02～10 mg·L-1.沼液实际样品的加标回收率范围为74.2％～102.9％.方法的检出限为2.8～21.0 μg·L-1.应用此方法对南京地区分别以猪粪、牛粪、鸡粪为发酵原料的3个沼气工程的沼液样品进行分析测定,结果表明在3种不同发酵原料的沼液环境中,不同频率地检出了四环素类和磺胺类抗生素,浓度范围为21.7～125.5μg·L-1.该方法具有准确可靠、快速简便等优点,可用于沼液中上述9种组分的同时测定.

Simultaneous Determination of 3 TCs and 6 SAs in Biogas Slurry by Solid Phase Extraction and High Performance Liquid Chromatography

A solid-phase extraction (SPE)-high performance liquid chromatography (HPLC) method has been developed for simultaneous determination of 3 tetracyclines (TCs) and 6 sulfonamides (SAs) in biogas slurry.The analytes were extracted by Na2EDTA,enriched and purified through HLB solid phase extraction column,and eluted with methanol,then detected by HPLC with a UV detector.The detection wavelength was 270 nm and the column temperature was 25 ℃,using isocratic elution process with acetonitrile 0.1 ％ acetic acid as the mobile phase to achieve baseline separations of these 9 analytes.The linearity range was 0.02-10 mg·L-1.The recoveries of standard-spiked real biogas slurry samples were 74.2％-102.9％.The limits of detection was 2.8-21.0 μg·L-1.The developed method was applied for analysis of samples collected from 3 biogas projects in Nanjing,which were fermented cow dung,pig dung and chicken dung,respectively.Results showed that TCs and SAs were detected in three different fermentation raw materials of biogas slurry,with the concentration range of 21.7-125.5 μg·L 1.This method is accurate and reliable and can be applied to the simultaneous determination of 3 TCs and 6 SAs in biogas slurry.