引用本文:梁晶,南淑清,张军,熊飚,申进朝.气相色谱/质谱法测定水中15种酞酸酯类化合物[J].环境监控与预警,2016,8(5):22-26
LIANG Jing, NAN Shu qing, ZHANG Jun, XIONG Biao, SHEN Jin chao.Determination of 15 Phthalic Acid Esters (PAEs) in Water by GC/MS[J].Environmental Monitoring and Forewarning,2016,8(5):22-26
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气相色谱/质谱法测定水中15种酞酸酯类化合物
梁晶,南淑清,张军,熊飚,申进朝
河南省环境监测中心,河南 郑州 450000
摘要:
采用固相萃取-气相色谱/质谱法测定水中15种酞酸酯类化合物,确定方法的最优条件为:依次用10 mL正己烷和丙酮混合溶剂(V/V=5∶1)、甲醇和空白试剂水活化C18固相萃取柱后,水样以5mL/min过柱萃取,再以8mL正己烷:丙酮(V/V=5∶1)混合溶剂洗脱后,浓缩至1mL,进气相色谱/质谱测定。该法的检出限为0.18~0.38μg/L,在0.50~20.0mg/L范围内线性良好,相关系数均>0.996。空白水样的加标回收率为71.8%~120%,相对标准偏差为1.73%~12.7%;实际废水水样的加标回收率为64.8%~135%,相对标准偏差为2.75%~18.0%。
关键词:    酞酸酯  固相萃取  气相色谱/质谱
DOI:
分类号:X832;O657.63
文献标识码:B
基金项目:国家高技术研究发展计划(863计划)(2013AA06A308)
Determination of 15 Phthalic Acid Esters (PAEs) in Water by GC/MS
LIANG Jing, NAN Shuqing, ZHANG Jun, XIONG Biao, SHEN Jinchao
Henan Environmental Monitoring Center, Zhengzhou, Henan 450000, China
Abstract:
The method was developed for the determination of fifteen phthalic acid esters in water by gas chromatography/mass spectrometry with solid phase extraction. The optimal conditions were discussed in this research. The C18solid phase extraction column was activated successively with 10 mL mixed solvent of hexane and acetone (V/V=5∶1), methanol, and blank water. The flow rate of sample was 5 mL/min. The eluting solvent was 8 mL mixed solvent of hexane and acetone (V/V=5∶1). The sample was concentrated to 1 mL, and then analyzed by gas chromatography /mass spectrometry. The detection limits of this method were from 0.18 to 0.38 μg/L, and the linearity was good from 0.50~20.0 mg/L with the correlation coefficients greater than 0.996. The recoveries of the spiked blank water samples were 71.8%~120%, and the relative standard deviations were 1.73%~12.7%. The recoveries of the actual water samples were 64.8%~135%, and the relative standard deviations were 2.75%~18.0%.
Key words:  Water  PAEs  Solid phase extraction  GC/ MS