Li Yanyan, Wei Guohui, Wang Xuedong
Key Laboratory of Pesticide & Chemical Biology of Ministry of Education, Central China Normal University, Wuhan, China.
J Sep Sci. 2007 Nov;30(16):2698-702. doi: 10.1002/jssc.200700188.
This paper describes the development of a new method using single-drop microextraction (SDME) and RP-HPLC for the determination of decabromodiphenyl ether (BDE-209) in water samples. The effects of SDME parameters such as extraction solvent, microdrop volume, extraction time, stirring speed, salt concentration, and sample pH on the extraction performance are investigated. Under optimal extraction conditions (extraction solvent, toluene; solvent drop volume, 3.0 microL; extraction time, 15 min; stirring speed, 600 rpm; no addition of salt and change of sample pH), the calibration curve was drawn by plotting peak area against a series of BDE-209 concentrations (0.001-1 microg/mL) in aqueous solution; the correlation coefficient (r) was 0.9998. The limit of detection was 0.7 ng/mL. The enrichment factor was 10.6. The precision of this method was obtained by six successive analyses of a 100 ng/mL standard solution of BDE-209, and RSD was 4.8%. This method was successfully applied to the extraction of BDE-209 from tap and East Lake water samples with relative recoveries ranging from 92.5 to 102.8% and from 91.5 to 96.2%, respectively, and the relative standard deviations (n = 3) were 4.4 and 2.2%. The proposed method is acceptable for the analysis of BDE-209 in water samples.
本文描述了一种采用单滴微萃取（SDME）和反相高效液相色谱（RP-HPLC）测定水样中十溴二苯醚（BDE-209）的新方法的开发。研究了萃取溶剂、微滴体积、萃取时间、搅拌速度、盐浓度和样品pH值等SDME参数对萃取性能的影响。在最佳萃取条件下（萃取溶剂为甲苯；溶剂滴体积为3.0微升；萃取时间为15分钟；搅拌速度为600转/分钟；不添加盐且不改变样品pH值），通过绘制峰面积与一系列水溶液中BDE-209浓度（0.001 - 1微克/毫升）的关系绘制校准曲线；相关系数（r）为0.9998。检测限为0.7纳克/毫升。富集因子为10.6。通过对100纳克/毫升的BDE-209标准溶液进行六次连续分析获得该方法的精密度，相对标准偏差（RSD）为4.8%。该方法成功应用于从自来水和东湖水样中萃取BDE-209，相对回收率分别为92.5%至102.8%和91.5%至96.2%，相对标准偏差（n = 3）分别为4.4%和2.2%。所提出的方法可用于分析水样中的BDE-209。
