高效液相色谱-荧光检测法测定大气细颗粒物(PM2.5〖KG-*5〗)中的双酚A

目的 建立大气细颗粒物(PM2.5)中双酚A 的高效液相色谱-荧光测定法,并用于成都市大气细颗粒物(PM2.5)中BPA的测定。方法 以玻璃纤维滤纸为滤料,用中流量PM2.5 采样器以100L/min的流速连续采样24h。滤纸样品经0.1%盐酸-甲醇超声提取后经C18小柱固相萃取,用0.1%氨水-甲醇洗脱,洗脱液调pH 2~3后,C18色谱柱(250mm×4.6mm,5μm)分离,荧光法检测(λex=227nm,λem=310nm)。结果 在0.001μg/ml~0.020μg/ml范围内回归方程为y=5.39×106x+5146,相关系数大于0.997;方法检出限为3.0×10-5μg/ml,定量限为1.1×10-4μg/ml,最低检出含量为200pg/m3(取样1/8分析),加标回收率为94.9%~104.8%,RSD为2.84%~9.23%。利用本法检测了20个成都市大气细颗粒物样品,测得双酚A含量范围在<200~4654pg/m3,平均含量为1455pg/m3。结论 本法灵敏度高,准确度好,检出限低,适用于大气中细颗粒物中双酚A的检测。成都市大气细颗粒物中双酚A的含量高于日美等发达国家以及我国北京、广州、香港,但低于印度的报道值。

Determination of bisphenol A in atmospheric fine particulate matter (PM2.5) by high performance liquid chromatography with fluorescence detection

Objective To establish a high performance liquid chromatography (HPLC) with fluorescence detection for the determination of bisphenol A (BPA) in atmospheric fine particulate matter (PM2.5),and to apply it to the determination of BPA in atmospheric PM2.5 collected from Chengdu,China. Methods Glass fiber filter paper was used as filter material,and a medium flowrate sampler was used to sample continuously for 24h at a flow rate of 100L/min.BPA in the filter paper sample was extracted ultrasonically with 0.1%hydrochloric acid-methanol,cleaned-up with C18 cartridge and eluted with 0.1%ammonia-methanol.After the pH of the sample solution was adjusted to 2-3 with hydrochloric acid,it was separated by C18 column,and detected by high performance liquid chromatography with fluorescence detection (Lex=227nm,Lem=310nm). Results The regression equation was y=5.39×106x+5146,with the correlative coefficient of 0.997.The detection limit was 3.0×10-5 mg/ml,and the quantitative limit was 1.1×10-4 mg/ml.The lowest detectable concentration was 200 pg/m3(for 1/8 filter paper sample),and the recoveries were 94.9%-104.8%with the RSDs of 2.84%-9.23%.BPA in 20 samples of atmospheric fine particles collected in Chengdu was determined by this method.The contents of BPA were in the range of 200-4654 pg/m3,with the average content of 1455 pg/m3. Conclusion This method has high sensitivity,good accuracy and low detection limit.It is suitable for the determination of bisphenol A in atmospheric fine particles (PM 2.5).The contents of bisphenol A in fine particulate matter in Chengdu are higher than those in developed countries such as Japan and the United States,as well as in Beijing,Guangzhou and Hong Kong,but lower than the reported value in India.