摘要
为测定污染土壤中的6种低残留喹诺酮类抗生素(氧氟沙星、培氟沙星、恩诺沙星、环丙沙星、诺氟沙星、恶喹酸),全面优化了一种联合加速溶剂萃取(ASE)、固相萃取(SPE)和高效液相色谱/三重四级杆质谱(HPLC/MSMS)3种检测技术的分析方法。样品采用甲醇和0.1 mol/L EDTA-McIlvaine缓冲液(1∶1)进行加速溶剂萃取,经Bond Elut Plexa型HLB固相萃取小柱富集纯化,土壤中6种喹诺酮类抗生素的基质效应因子控制在0.84~1.04。在0.2~100.0μg/L(以恶喹酸计)质量浓度范围内,目标化合物的线性关系良好(r>0.999),6种目标化合物的检出限为0.09~0.75μg/kg,加标回收率为60.9%~89.9%。该方法自动化程度和准确度较高,可极大程度地降低基质效应,提高测定方法的灵敏度,适用于土壤中喹诺酮类抗生素残留的检测。
A combination analysis method was developed for determination of six quinolone antibiotics(ofloxacin,pefloxacin,enrofloxacin,ciprofloxacin,norfloxacin and oxolinic acid)in contaminated soil by accelerated solvent extraction(ASE),solid phase extraction(SPE)and high performance liquid chromatography/tandem triple quadruple bar mass spectrometry(HPLC/MSMS).The analytes were extracted with methanol and 0.1 mol/L EDTA-McIlvaine buffer solution(1∶1),enriched and purified by bond elut plexa HLB solid phase extraction column,the matrix factor(MF)of six quinolones was controlled between 0.84 and 1.04 in soil.Good linearities of target compounds were realized in the range of 0.2 to 100.0μg/L(measured by oxolinic acid)with the correlation coefficients r>0.999.The limits of detection(MDL)were 0.09-0.75μg/kg,recovery rate ranged from 60.9%to 89.9%.The method was highly automatic and accurate,greatly reduced the matrix effect and improved the detection sensitivity,which was suitable for the determination of quinolone antibiotics residues in soil.
作者
杨静
YANG Jing(Fengxian Environmental Monitoring Station of Shanghai,Shanghai 200499,China)
出处
《中国环境监测》
CAS
CSCD
北大核心
2021年第1期156-164,共9页
Environmental Monitoring in China
关键词
加速溶剂萃取
固相萃取
高效液相色谱/三重四级杆质谱
喹诺酮类抗生素
accelerated solvent extraction
solid phase extraction
high performance liquid chromatography-tandem triple quadruple bar mass spectrometry
quinolone antibiotics
