摘要
建立了一种使用加速溶剂萃取(ASE)、固相萃取(SPE)联合超高效液相色谱/三重四极杆串联质谱(UPLC/MS/MS)测定沉积物中10种磺胺类抗生素的分析方法,分别考察了ASE中不同提取溶剂、温度、压力、萃取次数和SPE中不同上样体积对萃取效果的影响。样品采用甲醇和0.1 mol/L Mcllvaine缓冲溶液作为萃取溶剂,在萃取压力为10 MPa、萃取温度为80℃条件下重复萃取2次,用超纯水复溶至300 mL,经SAX-HLB串联固相萃取小柱进行富集纯化,定容后采用外标法定量分析。结果表明,10种磺胺类抗生素(SAs)在1~300μg/L范围内线性关系良好(R^(2)>0.994),方法检出限为0.034~0.396 ng/g;平均回收率介于67.8%~109.8%之间;相对标准偏差(RSD)介于1.76%~13.00%之间。该方法具有溶剂用量少、自动化程度高、操作简便、灵敏度高、重复性好等特点,可满足沉积物中SAs残留检测的要求,具有实际的应用前景。
This study established the combined use of accelerated solvent extraction(ASE),solid phase extraction(SPE),and ultra performance liquid chromatography/triple quadrupole tandem mass spectrometry(UPLC/MS/MS)for the determination of 10 sulfonamide antibiotics in sediments.For the analysis of ASE,we investigated the effects of different extraction solvents,temperatures,pressures,extraction times and solid phase extration(SPE)on the extraction efficiency.The sample was extracted with methanol and 0.1 mol/L Mcllvaine buffer as the extraction solvent.The extraction was repeated twice at an extraction pressure of 10 MPa and an extraction temperature of 80℃.After being reconstituted with ultrapure water to 300 mL,it was solidified by SAX-HLB.The phase extraction cartridge was used for enrichment and purification,and the external standard method was used for quantitative analysis after constant volume.The results showed that the 10 SAs antibiotics had a good linear relationship in the range of 1-300μg/L(R^(2)>0.994).The detection limit of the method was 0.034-0.396 ng/g.The average recovery rate was between 67.8%and 109.8%,and the relative standard deviation(RSD)was between 1.76%and 13.00%.The method has the characteristics of low solvent consumption,high degree of automation,simple operation,high sensitivity,and good repeatability.It can meet the requirements of SAs residue detection in sediments and has practical application prospects.
作者
张健威
梁延鹏
覃礼堂
曾鸿鹄
宋晓红
莫凌云
ZHANG Jianwei;LIANG Yanpeng;QIN Litang;ZENG Honghu;SONG Xiaohong;MO Lingyun(College of Environmental Science and Engineering,Guilin University of Technology,Guilin 541004;Guangxi Key Laboratory of Environmental Pollution Control Theory and Technology,Guilin 541004;Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area,Guilin 541004)
出处
《分析科学学报》
CAS
CSCD
北大核心
2023年第1期54-60,共7页
Journal of Analytical Science
基金
广西自然科学基金项目(2018GXNSFAA281186)
国家自然科学基金(51868012)
广西科技计划项目(桂科AD18126018)
广西“八桂学者”岗位专项经费资助。
关键词
加速溶剂萃取
固相萃取
超高效液相色谱-串联质谱
磺胺类抗生素
沉积物
Accelerated solvent extraction
Solid phase extraction
Ultra performance liquid chromatography/triple quadrupole tandem mass spectrometry
SAs antibiotics
Sediment
