固相微萃取-高效液相色谱联用测定水样中的痕量苯并(k)荧蒽

Determination of trace benzo(k) fluoranthene in water by SPME coupled with HPLC

研究了固相微萃取(SPME) 高效液相色谱(HPLC)联用测定水样中痕量苯并(k)荧蒽的的分析方法。对SPME的条件如萃取时间、萃取温度、离子强度、解吸方式、解吸溶剂、解吸时间和HPLC条件进行了优化,建立了SPME HPLC联用分析水样中痕量苯并(k)荧蒽的方法,并用于自来水、雨水和纯净水等实际水样的分析。SPME优化的条件为室温、搅拌速度1100r min、萃取时间30min、甲醇解吸溶剂、解吸时间2min。HPLC的条件为C18反相色谱柱、甲醇流动相、流速1mL min、紫外检测器、波长244nm,以峰高为测量信号。方法的线性范围为0～8.00μg L,检出限为0.014μg L,相对标准偏差(n=6)为6.7%,回收率为82.0%～104.2%。该方法适合于水样中痕量苯并(k)荧蒽的分析。

A method for the determination of trace benzo(k) fluoranthene in water was devel oped by using solid-phase microextraction (SPME) coupled with high-perforamnce liquid chromatography (HPLC). The experimental conditions of SPME, such as extr action time, extraction temperature, effect of ion strength, desorption time,de sorption solution, desorption mode, and the analytical conditions of HPLC were o ptimized. The SPME was then operated at room temperature, conditions were with t he stir rate of 1100 r /min, extraction time of 30 min, desorption time of 2 min,and methanol as the d esorptio n solution. Methanol was used as the mobile phase on the C18 reversed phas e chromatography column. The flow rate was 1 mL/min. The detection wavelength wa s 244 nm with the UV-Vis detector. The linear range of the method was from 0 to 8.0 μg/L with a detection limit of 0.014 μg/L, and the relative standard devi a tion (RSD%, n=6) of 6.7%. This method was used for the trace determination of benzo(k) fluoranthene in water sample, such as tap water, purified water and rain water, and the recovery was from 82.0% to 104.2%.