摘要
建立并优化了基于超高相液相色谱-三重四级杆串联质谱技术测定沉积物中壬基酚和双酚A含量的方法。沉积物样品经HLB-SPE萃取柱处理后,以甲醇-5 mmol甲酸铵为流动相,通过Agilent Eclipse Plus C18 RRHD超高效液相色谱柱进行分离和分析,选择电喷雾离子源,多反应监测负离子模式下进行测定。结果表明,壬基酚和双酚A在质量浓度5~100μg/L范围内均呈良好的线性关系,R^(2)≥0.99,检出限范围为0.066~0.14μg/L,平均回收率为88.9%~105%,精密度为2.97%~8.20%。方法的选择性、灵敏度及准确性均良好,可实现沉积物中壬基酚和双酚A含量的同时准确测定。
A method for determining the content of nonylphenol and bisphenol A in soil sediment using high-performance liquid chromatography mass spectrometry was established via optimizing various parameters,such as mobile phase,chromatographic column,mass spectrometry parameters.After extracting,the soil sediments were concentrated and purified by solid phase extraction.While,methanol-5 mmol/L ammonium formate was used as mobile phase for separating and analyzing by Agilent Eclipse Plus C18 RRHD ultra high performance liquid chromatography column,in which,the negative electrospray(ESI-)under multiple reaction monitoring(MRM)mode was detected.The results demonstrated that its detection limit range was 0.066~0.14μg/L and its linear range was 5~100μg/L with R^(2)≥0.99.especially,its average recovery range was 88.9%~105%and relative standard deviation range was 2.97%~8.20%This method presented a good selectivity,sensitivity,accuracy,and repeatability,which could meet the needs of accurate trace determination of nonylphenol and bisphenol A content in soil sediments.
作者
王安冬
赵明
周刚
祝永卫
WANG An-dong;ZHAO Ming;ZHOU Gang;ZHU Yong-wei(Analysis and Testing Center,Beijing University of Technology,Beijing 100124,China)
出处
《化学试剂》
CAS
2024年第6期77-82,共6页
Chemical Reagents
基金
新工科背景下的大型仪器设备开放共享的多元模式运行机制项目(JSWZ201801)。
关键词
壬基酚
双酚A
沉积物
高效液相色谱质谱联用
新污染物
nonylphenol
bisphenol A
soil sediment
liquid chromatography-mass spectrometry
emerging contaminant
