摘要
采用固相萃取结合高效液相色谱-串联质谱(HPLC-MS/MS)技术,建立了同时测定土壤中12种有机磷酸酯(OPEs)的方法。土壤样品经冷冻干燥、过筛后,加入丙酮-正己烷(1∶1,体积比)超声提取,经CNW⁃BOND Florisil SPE小柱净化后,进行HPLC-MS/MS分析,采用内标法定量。12种OPEs在0.1~100μg/L质量浓度范围内线性良好,相关系数(r^(2))均大于0.999,检出限为0.004~0.162 ng/g。在低、中、高3种加标水平下,平均加标回收率为67.0%~128%,相对标准偏差为1.5%~9.9%。利用该方法对20份土壤样本进行检测,12种目标化合物均有检出,OPEs总含量为5.36~55.2 ng/g(干重),平均值为23.7 ng/g(干重),中位数为25.0 ng/g(干重)。该方法灵敏度高,准确度和精密度良好,适用于土壤样品中OPEs的测定。
An effective analytical method was established for the determination of 12 organophos⁃phate esters(OPEs)in soil by solid phase extraction coupled with high performance liquid chromatog⁃raphy-tandem mass spectrometry(HPLC-MS/MS)in this paper.After freeze-drying and sieving,the soil samples were ultrasonically extracted with acetone-hexane(1∶1,by volume),then puri⁃fied with a CNWBOND Florisil SPE cartridge,and finally analyzed by HPLC-MS/MS.The internal standard method was used for quantification.There were good linear relationships for 12 OPEs in the concentration range of 0.1-100μg/L,with correlation coefficients(r^(2))greater than 0.999 and de⁃tection limits of 0.004-0.162 ng/g.The average recoveries at low,medium and high three spiked levels ranged from 67.0%to 128%,with relative standard deviations of 1.5%-9.9%.12 OPEs were detected simultaneously in 20 soil samples by the method established.All target compounds were detected with a total content of OPEs ranging from 5.36 to 55.2 ng/g(dry weight),the mean value of 23.7 ng/g(dry weight)and the median value of 25.0 ng/g(dry weight).This method is suit⁃able for the determination of OPEs in soil samples with sensitive and reliable results.
作者
王涛
张虹
周寒琳
林捷
童萍
贲玉婕
王耀强
韩永和
张勇
李家兵
WANG Tao;ZHANG Hong;ZHOU Han-lin;LIN Jie;TONG Ping;BEN Yu-jie;WANG Yao-qiang;HAN Yong-he;ZHANG Yong;LI Jia-bing(College of Carbon Neutral Modern Industry,College of Environmental and Resource Science,Fujian Normal University,Fuzhou 350117,China;Fujian Key Laboratory of Pollution Control and Resource Reuse,Fuzhou 350117,China;Fujian College Association Instrument Analysis Center,Fuzhou University,Fuzhou 350116,China;School of Environmental Science and Engineering,Southern University of Science and Technology,Shenzhen 518055,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第7期825-832,共8页
Journal of Instrumental Analysis
基金
福建师范大学高层次引进人才启动经费(Y0720304X13)
福建师范大学2023年大学生创新创业训练计划项目(cxxl-2023408)
福建省教育厅中青年教师教育科研项目(JAT190081)。
关键词
有机磷酸酯
土壤
固相萃取
高效液相色谱-串联质谱法
organophosphate esters
soil
solid phase extraction
high performance liquid chro⁃matography-tandem mass spectrometry
