摘要
目的建立同时测定水中25种半挥发性有机物的固相微萃取一气相色谱一质谱联用方法。方法通过自动固相微萃取仪,将固相微萃取纤维头浸入标准溶液和样品中直接萃取,选择合适的萃取纤维头,优化萃取温度、萃取时间、搅拌速率、解吸温度和时间等参数,在选定的条件下,目标组分经固相微萃取吸附、浓缩、解吸等步骤后进入气相色谱仪进行分离。分离后的组分进入质谱检测器,经全扫描定性,特征离子峰面积外标法定量。结果 25种半挥发性有机物在(0.5~5.0)μg/L具有良好的线性,其相关系数均>0.99,检出限范围(0.002~0.44)μg/L,回收率范围70.3%~119.0%,RSD范围4.0%~13.4%。利用该方法对北京市范围内10份生活饮用水进行了检测,目标组分均未检出。结论该方法操作简便、迅速,环境友好,具有较好的准确度和灵敏度,适用于水中25种半挥发性有机物的同时测定。
Objectives To establish a method for the determination of 25 semivolatile organic compounds in drinking water by micro-extraction gaschromatography─mass spectrometry. Methods Dipping the solid phase micro-extraction fiber of an automated solid phase micro-extraction（ SPME） instrument into standard solution or sample to extract target compounds. The parameters for SPME instrument,including the selection of fibre type,extraction temperature,extraction time,stir speed,desorbing temperature and the time,were optimized. Under selected conditions,samples were injected and separated by gas chromatography,qualified by full scan and quantified by the peak area with external standard. Results The linear ranges of the method was（ 0. 5 ~ 5. 0） μg/L,the correlation coefficient was greater than 0. 99. The detection limits of the method was in the range of（ 0. 002 ~ 0. 44） μg/L,the recovery rates was in the range of 70. 3% ~ 119. 0%,and the relative standard deviation was in the range of 4. 0% ~ 13. 4%. Conclusions This method was simple,rapid,accurate and sensitive and was suitable for detecting 25 semivolatile organic compounds in drinking water.
出处
《环境卫生学杂志》
2018年第4期340-344,349,共6页
JOURNAL OF ENVIRONMENTAL HYGIENE
关键词
固相微萃取
气相色谱-质谱法
饮用水
半挥发性有机物
solid phase micro-extraction
gas chromatography-mass spectrometry
drinking water
semivolatile organic compounds
