摘要
建立顶空固相微萃取结合气相色谱-三重四级杆质谱联用技术(HS-SPME-GC-MS/MS)对水中34种有机氯农药和氯苯类化合物检测的方法。探究萃取头类型、萃取时间、萃取温度及离子强度等条件对萃取效率的影响。实验结果表明采用二甲基硅氧烷/二乙烯基苯(PDMS/DVB)萃取纤维头、萃取时间为20min、萃取温度70℃、氯化钠(NaCl)加入量2.0g时,萃取效果较好。使用弱极性HP-5MS(固定相为5%苯基-甲基聚硅氧烷)毛细柱分离,三重四级杆全扫模式定性,动态多反应监测模式(dMRM)联合内标法定量,方法线性范围4~400ng/L,相关系数(R2)大于0.99,方法检出限为3.5~8.5ng/L,样品加标回收率为70.2%~108%,相对标准偏差(RSD)为0.98%~15.8%。
In this study,a method for the determination of 26 Organochlorine Pesticides(OCPs)and 8 chlorobenzenes(CBs)in water by HS-SPME-GC-MS/MS were established,to explore the influence of SPME fiber,extraction time,temperature and ion concentration on extraction efficiency.The results showed that the extraction effect was better when using the SPME fiber of poly(dimethysiloxane)/divinylbenzene(PDMS/DVB),the extraction time was 20min,the extraction temperature was 70℃,and the dosage of NaCl was 2.0g.Chromatographic separation on an HP-5MS chromatographic column,the compounds were analyzed under the dynamic multiple reaction monitoring(dMRM)mode and quantitated by internal standard method.The linearity of the method was good in the range of 4~400ng/L with a correlation coefficient(R2)over 0.99.The detection limits were from 3.5~8.5 ng/L,the average recovery rates of the samples were from 70.2%to 108%with RSD ranged from 0.98%to 15.8%.
作者
张洋阳
邵娟
杨存满
孟静
ZHANG Yang-yang;SHAO Juan;YANG Cun-man;MENG Jing(Nanjing University&Yancheng Environmental Detection Science&Technology Ltd.,Yangcheng,Jiangsu 224002,China)
出处
《四川环境》
2020年第2期111-119,共9页
Sichuan Environment
关键词
有机氯农药
氯苯类化合物
顶空固相微萃取
气相色谱-三重四级杆质谱联用
Organochlorine pesticides
chlorobenzenes
headspace solid phase micro-extraction
gas chromatography-triple quadrupole mass spectrometry
