固相萃取-气相色谱法测定饮用水中11种有机磷阻燃剂

Determination of 11 organophosphorus flame retardants in drinking water by solid phase extraction-gas chromatography-flame photometric detector method

目的 建立生活饮用水中11种有机磷阻燃剂（OPFRs）的固相萃取-气相色谱火焰光度（SPE-GC-FPD）测定方法,并与固相萃取-气相色谱氮磷检测器法（SPE-GC-NPD）进行比较。方法 采用oasis HLB固相萃取柱对生活饮用水中OPFRs进行提取和富集,气相色谱进行分离,火焰光度检测器上进行检测,以保留时间定性、外标法定量。结果 11种OPFRs线性范围238-6 250μg/L,线性相关系数（r）0.998-0.999,样品最低检出限73-263ng/L。低质量浓度级别加标回收率范围73%-122%;高质量浓度级别加标回收率范围55%-99%。平行样相对标准偏差（RSD）范围为0.8%-13.8%。与SPEGC-NPD法检测结果比较差异均无统计学意义（P值均〉0.05）。结论建立了SPE-GC-FPD测定生活饮用水中11种OPFRs的方法,该方法灵敏度、精密度较高,与常用有机磷农药互不干扰,适合日常生活饮用水中OPFRs残留检测。

Objective To establish a method to analyze 11 organophosphorus flame retardants （OPFRs） in drinking water by solid phase extraction-gas chromatography flame photometry detector （SPE-GC-FPD） method; to analyze OPFRs residues in drinking water and compare with solid phase extraction-gas chromatography-nitrogen and phosphorus detector （SPE GC- NPD） method. Methods The OPFRs in drinking water were extracted by solid phase extraction with oasis HI.B cartridge, followed by separation via gas chromatography and analysis in flame photometric detector. The OPFRs were identified by retention time and quantified by external standard method. Results The linear range of 11 OPFRs was from 238μg/L to 6 250 μg/ L,with coefficient of 0. 998-0. 999. The limit of detection in drinking water was from 73 ng/L to 263 ng/L. The recovery rate was from 73% to 122% at the low spiked level, and from 55% to 99% at the high spiked level. Relative standard deviation （RSD） was from 0.84% to 13.8%. A water sample was analyzed by SPE-G-C-FPD method and SPE-GC NPD method , no statistical difference was observed （all P〉0.05）. Conclusion A assay of 11 OPFRs in drinking water by SPE-GC-FPD method was established, which was sensitive and accurate, having no interference with common organic phosphorus pesticides. The assay was suitable for routine analysis of OPFRs in drinking water.