固相萃取-超高效液相色谱法测定养殖水体中磺胺类抗生素

建立了固相萃取-超高效液相色谱法串联测定养殖水体中8种磺胺类抗生素的分析方法。水样预处理后调p H值至6.0,以乙腈-二氯甲烷为提取液,添加氯化钠,以PEP柱与ODS-C18柱进行富集净化,采用超高效液相色谱进行定性定量分析,结果表明:8种磺胺类抗生素在水体中的检出限为0.01~0.03 mg/L,添加回收率为60.0%~89.0%,相对标准偏差为2.52%~7.10%。利用上述方法对不同水库(网箱)和池塘水样进行了检测,水体中磺胺类药物含量由高到低排序依次为:池塘养殖基地无公害养殖池塘网箱养殖基地。

Determination of Sulfonamide Antibiotics in Aquaculture Water by Solid-phase Extraction and Ultra Performance Liquid Chromatography

An analytical method was developed for the determination 8 kinds of sulfona mides antibiotics in aquaculture water. Adjusting pH value to 6.0, using acetonitrile - methylene chloride as extracting liquid, after adding sodium chloride, the pretreatment water sample was puriifed and concentrated by PEP and ODS-C18 after pretreatment, then qualitative and quantitative analysis were performed by UPLC. The results showed that the detective limitation values for 5 sulfona mides antibiotics in aquaculture water were obtained from 0.01 mg/L to 0.03 mg/L respectively, the recoveries were 60.0%-89.0% for water samples, and the relative standard deviation were 2.52%-7.10%. Taking above-mentioned method, sulfonamide antibiotics content in different reservoir (net cage) and the pond water sample were detected. The experimental results conifrmed that sulfonamide antibiotics content were arranged form high to low as follows: aquaculture pond, pollution-free aquaculture pond and net cage culture pond.