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
作者单位
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C<sub>18</sub>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
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 C<sub>18</sub>solid 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