摘要
为服务于抗生素类新污染物的水质环境监测需要,文章建立了固相萃取-高效液相色谱-三重四级杆质谱法,同步测定环境水体中磺胺类、喹诺酮类、大环内酯类等8种抗生素类新污染物。水样经固相萃取法富集净化后,用高效液相色谱-三重四级杆质谱法分离检测,根据化合物的保留时间和特征离子峰定性,外标法定量。结果表明:(1)目标物在液相色谱上得到有效的基线分离,保留时间稳定,在20~200 ng/L范围内标准曲线的相关系数R均在0.99以上;(2)8种抗生素类新污染物的方法检出限为0.65~3.12 ng/L;(3)经低浓度平行添加试验显示,方法的精密度为4.3%~10.9%,加标回收率为65%~98%。该研究建立的方法灵敏度高、适用性好,能够用于水质环境中磺胺嘧啶、磺胺醋酰、磺胺甲恶唑、磺胺甲氧哒嗪、磺胺噻唑、氧氟沙星、罗红霉素、螺旋霉素的监测分析。
To serve the needs of water quality and environment monitoring of new antibiotics pollutants,a solid-phase extraction high-performance liquid chromatography triple quadrupole mass spectrometry method was established to simultaneously determine eight new antibiotic pollutants,including sulfonamides,quinolones,and macrolides,in environmental water.After enrichment and purification by solid-phase extraction,the water sample was separated and detected by high-performance liquid chromatography triple quadrupole mass spectrometry.Qualitative analysis was performed based on the retention time and characteristic ion peaks of the compounds,while quantitative analysis was performed using external standard method.The results showed that:①The target substance obtained effective baseline separation on liquid chromatography,with stable retention time,and the correlation coefficients R of the standard curve were all above 0.99 in the range of 20~200 ng/L.②The detection limits of 8 new antibiotics was between 0.65 and 3.12 ng/L According to the low concentration parallel addition test,the precision of the method was 4.3%~10.9%,and the recovery rate of the added standard was 65%~98%.The method established in this study had high sensitivity and good applicability,and can be used for the monitoring and analysis of sulfamethoxazole,sulfamethoxazole,sulfamethoxazole,sulfamethoxazole,ofloxacin,roxithromycin,and spiramycin in water quality environments.
作者
魏莉
刘博
王铁龙
崔涤尘
张楠
刘嵩
李丹
王冬玲
WEI Li;LIU Bo;WANG Tielong;CUI Dichen;ZHANG Nan;LIU Song;LI Dan;WANG Dongling(Shenyang Ecological Environment Affairs Service Center,Shenyang 110167,China;Shenyang Academy of Environmental Sciences,Shenyang 110167,China;National Inspection and Testing Holding Group Liaoning Co.,Ltd,Shenyang 110000,China)
出处
《环境保护科学》
CAS
2024年第6期165-170,共6页
Environmental Protection Science
基金
辽宁省应用基础研究计划(青年专项)项目(2023JH2/101600011)。
关键词
新污染物
抗生素
固相萃取-高效液相色谱-三重四级杆质谱法
水质
环境监测
new pollutants
antibiotics
solid phase extraction high-performance liquid chromatography triple quadrupole mass spectrometry
water quality
environmental monitoring