SPE-HPLC/FLD法同时测定水中4种雌激素  

SPE-HPLC/FLD Method for the Determination of Four Estrogens in Water Samples

作　　者：付银杰[1,2] 高彦征[1] 董长勋[2] 刘娟[1] 凌婉婷[1] 

机构地区：[1]南京农业大学土壤有机污染控制与修复研究所,南京210095 [2]南京农业大学理学院,南京210095

出　　处：《农业环境科学学报》2012年第11期2296-2303,共8页Journal of Agro-Environment Science

基　　金：江苏省科技支撑计划(BE2011780);国家自然科学基金(21077056;41171193);中央高校基本科研业务费(KYZ201109)

摘　　要：研究建立了固相萃取(SPE)-高效液相色谱仪(HPLC)-荧光检测器(FLD)测定水体中4种雌激素(雌三醇、17β-雌二醇、炔雌醇和双酚A)的分析方法。水样过C18固相萃取柱净化浓缩,用5.00mL超纯水淋洗,15.00mL甲醇洗脱,洗脱液经氮气吹干后用50%甲醇溶解经HPLC-FLD测定;4种雌激素以甲醇/乙腈/水为流动相(体积比为25:30:45),经InertsilODS-SP-C1(8150mm×4.6mm,5μm)反相色谱柱分离,激发和发射波长分别为280nm和310nm,流速1.0mL.min-1,柱温40℃,进样量20μL,以保留时间定性、外标法定量。该方法的线性范围为5.00～1000.00μg.L-1,且相关性良好(R>0.9999),4种雌激素的仪器检出限为0.107～0.271μg.L-1,方法检出限为0.214～0.540ng.L-1。在自来水中添加不同浓度的雌激素混合标准溶液,测得溶液中4种物质的加标回收率除炔雌醇为55.71%～66.78%外,其余雌激素的加标回收率均大于85%,相对标准偏差RSD(n=5)均小于4%。该方法灵敏度高、检出限低、重复性和精密性良好,能有效去除基质干扰,可用于水体中痕量雌激素的分析测定。A solid phase extraction（SPE）-high performance liquid chromatography（HPLC）-fluorescence detection（FLD）method was established for the simultaneous determination of four estrogens（estriol,17β-estradiol,17а-ethynylestradiol,and bisphenol A）in water.Water samples was concentrated using a C18 solid phase extraction column,which was then consequently eluted with 5.00 mL ultrapure water and 15.00 mL methanol.Eluent was dried by nitrogen blow.The residue was then dissolved with 50% methanol solution,and determined by HPLC-FLD with the mobile phase of methanol/acetonitrile/wate（rvolume ratio of 25：30：45）at 1.0 mL.min-1,Inertsil ODS-SP-C1（8150 mm× 4.6 mm,5μm）reversed phase column at 40 ℃,excitation and emission of 280 nm and 310 nm,and injection volume of 20 μL.The linear range for the detection of test four estrogens was 5.00～1 000.00 μg.L-1 with correlations（r）higher than 0.999 9.Four estrogens detection limits of HPLC-FLD were 0.107～0.271 μg.L-1,the detection limits of SPE-HPLC/FLD were 0.214～540 ng.L-1.The recoveries of the four estrogens with SPE-HPLC/FLD were more than 85%,except 17а-ethynylestradiol of 60%,with relative standard deviations（RSD）（n=5）less than 4%.The method has high sensitivity,low detection limit,good reproducibility and precision,and may be used for the determination of trace amounts of estrogen in water environment.

关 键 词：高效液相色谱仪 荧光检测器 固相萃取 雌激素 水 

分 类 号：X830.2[环境科学与工程—环境工程]