光纤-固相微萃取耦合气相色谱法检测水中多溴联苯醚及其甲氧基衍生物

Determination of Polybrominated Diphenyl Ethers and Its Methoxylated Derivative in Water Samples Using Optical Fiber-Solid Phase Microextraction Couple with Gas Chromatography

建立了普通光纤-固相微萃取(Optical fiber-solid phase micro-extraction,OF-SPME)耦合气相色谱法分析水中多溴联苯醚(PBDEs)及其甲氧基衍生物(MeO-PBDEs)的方法。采用设计单因素实验结合二维交互实验进行条件优化实验,确定OF-SPME的最佳萃取条件为:搅拌速率1000 r/min,30%(V/V)甲醇,温度40℃,萃取90 min。13种PBDEs和5种MeO-PBDEs在3个不同加标浓度下的相对标准偏差分别为1.3%～10.3%,0.1%～5.0%和1.8%～14.0%;方法检出限在0.48～1.94 ng/L之间;在1.5～60 ng/L浓度范围内,其线性相关系数R2>0.9954。将本方法应用于生活污水中PBDEs和MeO-PBDEs的加标测定,在3个加标浓度下其相对标准偏差分别为0.3%～7.4%,0.3%～9.9%和1.9%～13%。本方法是一种可用于自然水体或者实验室PBDEs暴露水样中PBDEs和MeO-PBDEs分析的廉价、便捷、高效的技术手段。

Based on optical fiber-solid phase micro-extraction （OF-SPME） followed by gas chromatography （GC）, a novel method for the analysis of polybrominated diphenyl ethers （PBDEs） and methoxylated PBDE metabolites（MeO-PBDEs） in aqueous samples had been developed. Using both of single factor tests and 2-level factorial design, the optimized experimental conditions were determined to be extraction of 90 min with stirring rate of 1000 r/min, temperature of 40 ℃, methanol addition of 30% （ V/V）, and without salt addition. Pression of the method, established at three concentration levels of spiked water, was 1. 3%- 10.3% 0.1%-5.0% and 1.8%-14.0% RSD, respectively. The detection limits of the proposed method varied from 0.48 to 1.94 ng/L. The response was found to be linear in range of 1.5 -60 ng/L, with correlation coefficient （R2） better than 0. 995 for all the compounds. The pression was determined to be 0.3% -7.4%, 0.3% -9.9% and 1.9%-13% RSD in three concentration levels of spiked wastewater. OF- SPME was a cost-less, promising and effective method for the analysis of trace-level PBDEs and MeO-PBDEs in natural water or laboratory water from PBDEs exposure experiment.