摘要
文中建立了利用全自动固相萃取仪(Fotector 02HT)对水中多环芳烃经全自动固相萃取后用气相色谱质谱分析的检验方法。水样中有机化合物被C18固相萃取柱吸附,用二氯甲烷洗脱,洗脱液经浓缩,气相色谱毛细柱分析各个组分后,以质谱作为检测器,进行水中有机物测定。通过目标组分的质谱图和保留时间与计算机谱库中质谱图和保留时间对照进行定性,每个定性出来的组分的浓度取决于其定量离子与内标物定量离子的质谱响应之比。各样品中含已知浓度的内标化合物,用内标矫正程序测定。水样的检出限均低于1.0ng/mL,精密度在5.6%~11.5%之间,加标回收率92.4%~109.5%,相关系数在0.9997~0.9999,线性关系很好。通过该方法,可满足生活饮用水卫生标准有机物指标中16种多环芳烃指标检测要求,同时对其他的半挥发性进行定性或者定量检测,以满足突发公共卫生事件的检测要求。
In this paper,a method for the determination of polycyclic aromatic hydrocarbons(PAHs)in water by gas chromatography-mass spectrometry(GC-MS)after full-automatic solid phase extraction(FOTECTOR 02HT)was established.The organic compounds in the water sample were adsorbed by C18 SPE column and eluted by dichloromethane.After the eluent was concentrated,each component was analyzed by GC capillary column,and the organic compounds in water were determined by mass spectrometry as detector.The mass spectrum and retention time of the target component were compared with those in the computer spectrum library.The concentration of each component was determined by the ratio of the mass spectrum response of its quantitative ions to the quantitative ions of internal standard.The known concentration of internal standard compounds in each sample was determined by internal standard correction procedure.The detection limits of water samples were lower than 1ng/mL,the precision was 5.6%~11.5%,the recoveries were 92.4%~109.5%,the correlation coefficient was 0.9997~0.9999,and the linear relationship was good.This method can meet the detection requirements of 16 kinds of PAHs in the organic indicators of"Sanitary Standards for Drinking Water",and at the same time,qualitative or quantitative detection of other semi-volatiles can be carried out to meet the detection requirements of public health emergencies.
作者
杨惟喜
YANG Wei-Xi(Quality Inspection Institute of Nanping,Nanping 353000,Fujian,China)
出处
《质量技术监督研究》
2021年第4期11-14,共4页
Quality and Technical Supervision Research
关键词
多环芳烃
气相色谱质谱分析
全自动固相萃取
Polyeyclic Amatic Hydiocarbons
GC-MS
Automatic solid-phase extraction
