固相微萃取/气相色谱法检测甲基膦酸酯和磷酸酯

固相微萃取/气相色谱法检测甲基膦酸酯和磷酸酯

王一龙¹,²，曾昭睿², 王朝领²

1. 武汉理工大学理学院，武汉 430070； 2. 武汉大学化学与分子科学学院，武汉 430072

收稿日期:2006-10-23 修回日期:1900-01-01 出版日期:2007-07-26 发布日期:2007-07-26
通讯作者: 王一龙

Determination of Methylphosphonates and Phosphates in Air Samples Using Solidphase Microextraction Coupled with Gas Chromatography

WANG Yilong¹，², ZENG Zhaorui², WANG Chaoling²

1. School of Sciences, Wuhan University of Science and Technology, Wuhan 430070, China; 2. College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China

Received:2006-10-23 Revised:1900-01-01 Online:2007-07-26 Published:2007-07-26
Contact: WANG Yilong

摘要/Abstract

摘要： 采用溶胶凝胶方法制备的聚甲基苯基乙烯基硅氧烷/羟基硅油固相微萃取探头联用气相色谱对空气中的甲基膦酸酯和磷酸酯进行分析. 优化了固相微萃取的过程和热解析过程. 该探头的萃取能力强于3种商用固相微萃取探头. SPMEGC方法的检出限低（27.2~28.3 μg／L），重现性好（4.7~6.8%），线性范围为0.029 2~0.292 mg／L.对空白的空气样品进行标准加入回收实验，3种化合物甲基膦酸二甲酯、磷酸三甲酯和磷酸三丁酯的回收率分别为94.7%, 89.3%和 93.2%.

关键词: 溶胶凝胶技术, 聚甲基苯基乙烯基硅氧烷/羟基硅油, 固相微萃取, 甲基膦酸酯, 磷酸酯

Abstract: A solgelderived poly（methylphenylvinylsiloxane)(PMPVS)/hydroxy terminated silicone oil (OHTSO) solidphase microextraction fiber coupled with gas chromatography (GC) was developed to determine methylphosphonates and phosphates in air samples. The extraction and desorption parameters influencing on solidphase microextraction (SPME) process were optimized. Compared with three comme rcial SPME stationary phases, this fiber shows the best selectivity and sensitivity towards these compounds. The detection limits of this method varied from 27.2 to 28.3 μg／L, and the relative standard deviations (n=5) for these compounds were found to be from 4.7% to 6.8%. The linearity range was one order of magnitude. For blank air samples, standard additional experiment was used, the recoveries of three compounds, dimethy methyl phosphonate, trimethyl phosphate, tributyl phosphate were 94.7%,89.3% and 93.2%, respectively.

Key words: solgel technology, poly（methylphenylvinylsiloxane)/hydroxyterminated silicone oil, solidphase microextraction, methylphosphonates, phosphates

中图分类号:

O657

王一龙,，曾昭睿, 王朝领. 固相微萃取/气相色谱法检测甲基膦酸酯和磷酸酯[J]. J4, 2007, 45(04): 661-664.

WANG Yilong，, ZENG Zhaorui, WANG Chaoling. Determination of Methylphosphonates and Phosphates in Air Samples Using Solidphase Microextraction Coupled with Gas Chromatography[J]. J4, 2007, 45(04): 661-664.