超声溶剂萃取-气相色谱-质谱法测定PM2.5中16种多环芳烃
Determination of 16 polycyclic aromatic hydrocarbons in PM2.5 by ultrasonic solvent extraction-gas chromatography-mass spectrometry
张瑞 1杨妍1
作者信息
- 1. 郑州市疾病预防控制中心理化检验所,河南郑州 450007
- 折叠
摘要
目的 建立超声溶剂萃取-气相色谱-质谱联用技术(GC-MS)同时测定雾霾中16种多环芳烃(PAHs)的方法.方法 取1/4滤膜样品,剪碎后置于离心管中,加入3.5 mL正己烷浸没滤膜,冰水浴超声60 min后4 500r/min离心5 min,取1.0 mL上清液,GC-MS测定.结果 在0.2～10 μg/mL浓度范围内,线性关系良好,相关系数(r)为0.998 3～0.999 3.在选择离子扫描模式下,检出限为0.151～0.220ng/m3(以采集144 m3空气计),低、中、高3个水平的加标浓度的回收率范围为80.9％～99.8％,6次样品平行测定结果计算相对标准偏差在1.38％～3.92％.结论 该方法操作简单、重现性好、灵敏度高、定性定量准确,适用于空气中16种多环芳烃的大批量检测.
Abstract
Objective To establish a method for the determination of 16 polycyclic aromatic hydrocarbons(PAHs)in PM2.5 by ultrasonic extraction-gas chromatography-mass spectrometry(GC/MS).Methods One fourth of filter membrane was cut into pieces and placed in a centrifuge tube;3.5 mL of n-hexane was added to soak the filter membrane,and ultrasound was performed at 0℃ for 60 minutes.After that,centrifugation was performed at 4 500 r/min for 5 minutes.Then,1.0 mL of supernatant was taken,and GC-MS was used for the determination.Results The method had a good linear relationship in the range of 02-10 μg/mL,with a correlation coefficient(r)was between 0.998 3-0.999 3.Under the selected ion monitor(SIM)mode,the limits of quantification(LOQ)were from 0.151-0.220 ng/m3(the sampled volume of air was 144 m3).The recoveries at low,medium and high concentration levels were between 80.9％-99.8％.The relative standard deviation values(RSDs)were between 1.38％-3.92％with 6 times sample test.Conclusions This method is easy to operate and has high sensitivity,good reproducibility and more accurate qualitative quantification.It is suitable for mass detection of 16 PAHs in the PM2.5.
关键词
气相色谱-质谱法/多环芳烃/PM2.5/超声溶剂萃取Key words
Gas chromatography-mass spectrometry/Polycyclic aromatic Hydrocarbons/PM25/Ultrasonic solvent extraction引用本文复制引用
出版年
2024
NETL
NSTL
万方数据