固相萃取-高效液相色谱-串联质谱法同时测定土壤中氟喹诺酮、四环素和磺胺类抗生素_临床医学论文.docVIP

固相萃取-高效液相色谱-串联质谱法同时测定土壤中氟喹诺酮、四环素和磺胺类抗生素_临床医学论文 固相萃取-高效液相色谱-串联质谱法同时测定土壤中氟喹诺酮、四环素和磺胺类抗生素_临床医学论文 作者：马丽丽 郭昌胜 胡伟 沙健 朱兴旺 阮悦斐 王玉秋 【摘要】 建立了固相萃取-高效液相色谱-串联质谱法同时检测土壤中氟喹诺酮类、四环素类和磺胺类18种抗生素的分析方法。土样经含50%乙腈的磷酸盐缓冲液(pH=3)提取后，以SAX-HLB串联小柱净化富集，在HPLC/MS/MS多反应监测模式下进行定性及定量分析。添加浓度为200和50 μg/kg时，土壤中氟喹诺酮类、四环素类、磺胺类的加标回收率分别为67.2%~89.0%，62.2%~85.4%和55.8%~97.4%；其相对标准偏差为1.1%~17.2%。以3倍信噪比估算出氟喹诺酮类、四环素类、磺胺类的检出限分别为3.4~8.9 μg/kg，0.56~0.91 μg/kg和0.07~1.85 μg/kg。应用此方法检测6种不同类型土壤样品，结果表明，污灌区土壤中检出有抗生素，浓度为1.72~119.6 μg/kg。 【关键词】 氟喹诺酮；四环素；磺胺；固相萃取；高效液相色谱串联质谱；土壤 Abstract An analytical method was developed for the simultaneous extraction and determination of eighteen fluoroquinolones (FQs)，tetracyclines (TCs) and sulfonamides (SAs) antibiotics from soils using solid phase extraction and liquid chromatography tandem mass spectrometry.Soil sample was firstly extracted by phosphate buffer at pH 3 in combination with 50% of organic modifier acetonitrile，then purified and concentrated by SAX and HLB column.Qualitative and quantitative analysis were carried out for the analyte under the MRM mode after the chromatography separation on Kromasil C18 (250 mm×4.6 mm，5 μm) column.The range of recoveries (in percent) for FQs，TCs，SAs，in the soil matrix was 67.20%-88.98%，62.23%-85.36%，55.76%-97.37% with 1.1%-17.2% of relative standard deviation respectively in two different concentrations.The limits of quantification (LOQ，S/N=3) were 3.36-8.88 μg/kg，0.56-0.91 μg/kg and 0.07-1.85 μg/kg for FQs，TCs and SAs，respectively.This method was successfully used to detect 18 antibiotics in 6 soil samples with different land types in Tianjin.Results showed some of the antibiotics in the arable soil were detected，with concentrations of 1.72-119.57 μg/kg. 　　Keywords Fluoroquinolones；Tetracyclines；Sulfonamides；Solid phase extraction；High performance liquid chromatography-tandem mass spectrometry；Soil 　　1 引言 　　抗生素广泛应用于人类及动物疾病的防治。据报道，进入动物体内的抗生素有相当一部分随粪、尿等排泄物排出[1]，而粪便、尿液又作为有机肥大量施用于农田，造成抗生素在土壤中不断累积。部分进入污水处理厂的抗生素并不能完全被去除[2~5]，它们又随着终水排放进入环境中。当受污染