Basheer Chanbasha, Lee Hian Kee
Department of Chemistry, National University of Singapore, Singapore 117543, Republic of Singapore.
J Chromatogr A. 2004 Aug 27;1047(2):189-94. doi: 10.1016/j.chroma.2004.06.130.
A porous polypropylene hollow fiber membrane (HFM)-protected solid-phase microextraction (HFM-SPME) procedure in conjunction with gas chromatography/mass spectrometric analysis for use in the determination of triazine herbicides in bovine milk samples is described. A 65-microm polydimethylsiloxane-divinylbenzne (PDMS-DVB) SPME fiber was protected by an HFM. HFM-SPME experimental parameters such as fiber type, extraction time, extraction temperature and salt concentration were investigated and optimized. The relative standard deviations for the reproducibility of the optimized HFM-SPME method varied from 4.30 to 12.37%. The correlation coefficients of the calibration curves were between 0.9799 and 0.9965 across a concentration range of 0-200 microg l(-1). The method detection limits for triazines in bovine milk were in the range of 0.003-0.013 microg l(-1) and limits of quantification were in the range of 0.006-0.021 microg l(-1). The suitability of HFM-SPME was extended to the analysis of the herbicides in sewage sludge samples. The results demonstrate that HFM-SPME was an efficient pretreatment and enrichment procedure for complex matrices.
本文描述了一种多孔聚丙烯中空纤维膜（HFM）保护的固相微萃取（HFM-SPME）方法，该方法结合气相色谱/质谱分析用于测定牛奶样品中的三嗪类除草剂。一根65微米的聚二甲基硅氧烷-二乙烯基苯（PDMS-DVB）SPME纤维由HFM保护。对HFM-SPME的实验参数如纤维类型、萃取时间、萃取温度和盐浓度进行了研究和优化。优化后的HFM-SPME方法重现性的相对标准偏差在4.30%至12.37%之间。在0-200微克/升的浓度范围内，校准曲线的相关系数在0.9799至0.9965之间。牛奶中三嗪类除草剂的方法检测限在0.003-0.013微克/升范围内，定量限在0.006-0.021微克/升范围内。HFM-SPME的适用性扩展到污水污泥样品中除草剂的分析。结果表明，HFM-SPME是一种用于复杂基质的高效预处理和富集方法。
