摘要
建立了卤水中有机物的固相萃取-气相色谱/质谱(SPE-GC/MS)结合保留指数的分析方法。用石墨化碳黑柱对盐湖卤水中的有机物进行富集,采用GC-MS,以扫描离子检测模式(SCAN),选择离子检测模式(SIM)和保留指数法进行检测。考察了样品的pH值、洗脱剂种类、洗脱剂用量等因素,并对实验条件进行了优化。同时采用氘标记化合物氘代萘和1,3-二硝基苯-D4进行回收率实验,平均回收率在85.00%～91.70%之间,相对标准偏差(RSD)为2.32%～8.04%;且氘代萘和1,3-二硝基苯-D4分别在0.1～1mg/L和1～2mg/L范围内线性良好,相关系数R分别为0.9964和0.9957。利用优化的方法可一次检测出盐湖卤水中49种有机物,具有简便快捷、准确等优点。
A method was developed for the determination of organic compounds in saline water by solid-phase extraction-gas chromatography/mass spectrometry（SPE-GC/MS） combined with retention indices.The SPE preconcentration was performed on commercial graphitized black extraction cartridges,and GC-MS determination was operated in scan and selective ion monitoring（SIM） mode.Some important influence factors including sample acidity,eluent species and eluent volume were studied.Recovery studies using Naphthalene-D8 and 1,3-Dinitrobenze-D4 showed that the average recoveries of the method were in the range from 85.00% to 91.67% with the relative standard deviations（RSDs） from 2.32% to 8.04%.The linearity of the standards was in the range of 0.1～1 mg/L and 1～2 mg/L with a good linear correlation coefficient（R=0.9964 and R=0.9957）,respectively.49 organic compounds in saline water were successfully identified and quantified using the optimized method,which demonstrated the developed method was simple,sensitive and accurate in determining the organic compounds in saline water.
出处
《分析科学学报》
CAS
CSCD
北大核心
2011年第6期705-709,共5页
Journal of Analytical Science
基金
国家"十一五"支撑计划项目(No.2006BAB09B07)
青海省科技厅重点攻关项目(No.2008-G-106)
关键词
固相萃取
石墨化碳黑柱
盐湖卤水
保留指数
气相色谱-质谱
Solid-phase extraction
Graphitized carbon black extraction cartridges
Saline water
Retention indices
Gas chromatography-mass spectrometry
