摘要
建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时检测地表水中10种磺胺类抗生素的分析方法。过滤后的水样用稀H2SO4调节pH至6.0,经HLB固相萃取柱富集净化,依次用乙酸乙酯-甲醇(1∶1,V/V)、氨水-甲醇(3∶100,V/V)进行洗脱,采用超高效液相色谱-串联质谱法测定,外标法进行定量。结果表明,10种目标物在1~500μg/L范围内呈现良好的线性关系,相关系数均大于0.999,方法检出限在0.12~0.84ng/L范围。对水样进行低、中、高3个浓度水平加标实验,10种目标物的加标回收率分别为81.90%~93.69%、77.94%~96.83%、84.14%~104.98%,相对标准偏差小于8.1%。本研究所建立的方法具有操作简单、灵敏度高、重现性好等特点,能够快速、准确、可靠地测定地表水水样中残留的10种磺胺类抗生素。
A method was developed for the simultaneous determination of 10 sulfonamide antibiotics in surface water using solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS).The filtered water samples were adjusted to pH=6.0 by sulfuric acid,enriched and cleaned-up by HLB solid-phase extraction cartridge,then eluted by ethyl acetate-methanol(1∶1,V/V)and ammonia-methanol(3∶100,V/V).The target compounds were confirmed and quantified by UPLC-MS/MS with external standard method.The results showed that the calibration curves of the 10 antibiotics showed good linearity in the range of 1-500μg/L with the correlation coefficients larger than 0.999.The limits of detection ranged from 0.12-0.84 ng/L.The recoveries of three spiked levels of samples were 81.90%-93.69%for low concentration,77.94%-96.83%for medium concentration and 84.14%-104.98%for high concentration with the relative standard deviations less than 8.1%.The proposal method is suitable for quickly,accurately and reliably analyzing 10 sulfonamide antibiotics in surface water.
作者
庞昕瑞
曾鸿鹄
梁延鹏
覃礼堂
莫凌云
PANG Xin-rui;ZENG Hong-hu;LIANG Yan-peng;QIN Li-tang;MO Ling-yun(College of Environmental Science and Engineering,Guilin University of Technology,Guilin 541004;Guangxi Key Laboratory of Environmental Pollution Control Theory and Technology,Guilin University of Technology,Guilin 541004;Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area,Guilin University of Technology,Guilin 541004)
出处
《分析科学学报》
CAS
CSCD
北大核心
2019年第4期461-466,共6页
Journal of Analytical Science
基金
广西自然科学基金(No.2018JJ150039)
国家自然科学基金(No.51578171)
广西“八桂学者”岗位专项经费资助
广西科技计划(桂科AD18126018)
关键词
超高效液相色谱-串联质谱
固相萃取
磺胺类抗生素
地表水
Ultra-high performance liquid chromatography-tandem mass spectrometry
Solid-phase extraction
Sulfonamide antibiotics
Surface water
