中国环境监测
中國環境鑑測
중국배경감측
ENVIRONMENTAL MONITORING IN CHINA
2014年
5期
73-76
,共4页
葛璇%刘莉%王明泉%孙韶华%贾瑞宝
葛璇%劉莉%王明泉%孫韶華%賈瑞寶
갈선%류리%왕명천%손소화%가서보
液相色谱-串联质谱法%固相萃取%水%雌激素
液相色譜-串聯質譜法%固相萃取%水%雌激素
액상색보-천련질보법%고상췌취%수%자격소
LC-MS-MS%solid-phase extraction%water%estrogens
建立了固相萃取-液相色谱-串联质谱组合联用技术同时测定地表水、饮用水和污水处理厂出厂水中的5种雌激素(17β-雌二醇、雌三醇、雌酮、17α-炔雌醇、己烯雌酚)的方法。水样经过全自动固相萃取仪富集,以OASIS HLB柱为萃取柱,甲醇为洗脱剂,用液相色谱-串联四极杆质谱联用仪分析定量。分别在0?5~8、5~80μg/L范围内线性良好,相关系数为0?995~0?998。17β-雌二醇、雌三醇、17α-炔雌醇的检出限均为5μg/L,雌酮与己烯雌酚的检出限为0?5μg/L。5种雌激素的纯水加标回收率为63?6%~120?2%,地表水加标回收率为59?8%~91?5%,自来水加标回收率为55?3%~92?1%,精密度为3?7%~10?7%,该方法简单、可靠,可用于水中雌激素类污染物的同时测定。
建立瞭固相萃取-液相色譜-串聯質譜組閤聯用技術同時測定地錶水、飲用水和汙水處理廠齣廠水中的5種雌激素(17β-雌二醇、雌三醇、雌酮、17α-炔雌醇、己烯雌酚)的方法。水樣經過全自動固相萃取儀富集,以OASIS HLB柱為萃取柱,甲醇為洗脫劑,用液相色譜-串聯四極桿質譜聯用儀分析定量。分彆在0?5~8、5~80μg/L範圍內線性良好,相關繫數為0?995~0?998。17β-雌二醇、雌三醇、17α-炔雌醇的檢齣限均為5μg/L,雌酮與己烯雌酚的檢齣限為0?5μg/L。5種雌激素的純水加標迴收率為63?6%~120?2%,地錶水加標迴收率為59?8%~91?5%,自來水加標迴收率為55?3%~92?1%,精密度為3?7%~10?7%,該方法簡單、可靠,可用于水中雌激素類汙染物的同時測定。
건립료고상췌취-액상색보-천련질보조합련용기술동시측정지표수、음용수화오수처리엄출엄수중적5충자격소(17β-자이순、자삼순、자동、17α-결자순、기희자분)적방법。수양경과전자동고상췌취의부집,이OASIS HLB주위췌취주,갑순위세탈제,용액상색보-천련사겁간질보련용의분석정량。분별재0?5~8、5~80μg/L범위내선성량호,상관계수위0?995~0?998。17β-자이순、자삼순、17α-결자순적검출한균위5μg/L,자동여기희자분적검출한위0?5μg/L。5충자격소적순수가표회수솔위63?6%~120?2%,지표수가표회수솔위59?8%~91?5%,자래수가표회수솔위55?3%~92?1%,정밀도위3?7%~10?7%,해방법간단、가고,가용우수중자격소류오염물적동시측정。
A liquid chromatography-mass spectrometric ( LC-MS-MS ) method was established for the determination of five estrogens in surface water , drinking water and waste water. The sample was enriched with by solid-phase extraction column, extracted with methanol, evaporated by nitrogen, redissolved by acetonitrile/water(3∶2,V/V) and then analyzed by LC-MS-MS. Under the optimal conditions, good linearities were obtained in the range of 0?5-8 μg/L and 5-80 μg/L with correlation coefficients of 0?995-0?998. The limits of 17B-estradiol, estriol and 17α-ethiny lestradiol were all 5 μg/L and the limits of estrone and diethylstilbestrol were all 0?5μg /L. The recoveries of five estrogens in pure water,surface water and drinking water were 63?6%-120?2%, 59?8%-91?5% and 55?3%-92?1%. The relative standard deviations ranged from 3?7% to 10?7%. The method was simple and reliable and it could be used to determinate five estrogens in water at the same time.