固相萃取-气相色谱/质谱法测定水中6种有机磷酸酯类阻燃剂和增塑剂

Determination of Organophosphorus Flame Retardants and Plasticizers in Environmental Water by Solid Phase Extraction Coupled with Gas Chromatography/Mass Spectrometry

采用C18固相萃取小柱富集环境水样中6种常见的有机磷酸酯类阻燃剂和增塑剂,经气相色谱/质谱（选择离子扫描模式）检测,内标法定量,优化了固相萃取和气相色谱质谱检测参数。磷酸三（丁氧乙基）酯二次回归相关系数大于0.999,定量限为32ng/L。其余磷酸三丁酯、磷酸三（2-氯乙基）酯、磷酸三（2-氯异丙基）酯、磷酸三（1,3-二氯异丙基）酯和磷酸三苯酯5种有机磷酸酯组分在10~800μg/L浓度范围线性相关系数大于0.999,定量限介于1.1~4.1ng/L。纯水加标样品中6种组分回收率范围为73%~112%,相对标准偏差范围为1.2%~12.9%。应用该方法分析了太湖、长江和自来水样品,均检出多种有机磷酸酯组分,且太湖中浓度水平高于长江。实际样品中6种组分的加标回收率范围为83%~146%,相对标准偏差范围为0.9%~15.1%。

A method for determination of 6 organophosphorus flame retardants and plasticizers in environmental water were described. Target compounds were extracted using solid phase extraction（SPE） cartridges, separated by GC and detected with MS. Phenanthrene-d10 was used as an internal standard（IS）. C18 cartridge was used to SPE. And important SPE parameters were optimized. The regression coefficient of tris（2-butoxyethyl） phosphate （TBEP） was 0. 9996, limit of quantitation （LOQ） of TBEP was 32 ng/L （S/N ≥ 10）. The linear regression coefficients of the other 5 target compounds ranged from 0. 9991 to 0. 9998, LOQs of the other 5 target compounds varied between 1.1 and 4. 1 ng/L. Recoveries of spiked pure water varied from 73 % to 112 % with RSDs of 1.2-12.9 %. This method was successfully applied to water samples from Taihu Lake, Changjiang River and tap water. Recoveries of spiked samples varied from 83 %to 146 % with RSDs varied from 0.9 % to 15.1%. The target compounds were all detected in Taihu lake sample and 4 compounds detected in Yangtze river sample. The total concentration of 6 compounds in Taihu Lake was larger than that in Yangtze river.