Analysis of free estrogens and their conjugates in sewage and river waters by solid-phase extraction then liquid chromatography-electrospray-tandem mass spectrometry

被引:101
作者
Gentili, A [1 ]
Perret, D [1 ]
Marchese, S [1 ]
Mastropasqua, R [1 ]
Curini, R [1 ]
Di Corcia, A [1 ]
机构
[1] Univ Roma La Sapienza, Dipartimento Chim, I-00185 Rome, Italy
关键词
column liquid chromatography; solid-phase extraction; electrospray tandem mass spectrometry; estrogens in sewage and surface water;
D O I
10.1007/BF02490242
中图分类号
Q5 [生物化学];
学科分类号
071010 [生物化学与分子生物学]; 081704 [应用化学];
摘要
'Free' steroidal estrogens have been identified as compounds possibly responsible for endocrine-disruption of aquatic fauna populating rivers in which municipal sewage-treatment plants (STP) discharge their effluents. Natural and synthetic estrogens are excreted, as glucuronides and sulfates, by man, in the urine but these are bioconverted back to the unconjugated forms in wastewater discharges. For this reason we have developed a sensitive analytical procedure, without derivatization, for identification and quantitation of conjugated and free estrogens in surface and waste waters. The hormones were extracted and fractionated, by use of Carbograph cartridges, into neutral and acid fractions which were then analyzed by liquid chromatography-tandem mass spectrometry Recoveries were between 66 and 100% and limits of detection (LOD) between 15.0 and 0.003 ng L-1, depending on the compound and the water matrix. When this methodology was applied to real sewage and river water we could measure the main free estrogens at ng L-1 levels. Among the conjugates we always observed the presence of estrone 3-sulfate (at levels between 8.0 and 0.5 ng L-1).
引用
收藏
页码:25 / 32
页数:8
相关论文
共 19 条
[1]
ESTROGEN CONJUGATES IN LATE-PREGNANCY FLUIDS - EXTRACTION AND GROUP SEPARATION BY A GRAPHITIZED CARBON-BLACK CARTRIDGE AND QUANTIFICATION BY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY [J].
ANDREOLINI, F ;
BORRA, C ;
CACCAMO, F ;
DICORCIA, A ;
SAMPERI, R .
ANALYTICAL CHEMISTRY, 1987, 59 (13) :1720-1725
[2]
Analysis and occurrence of estrogenic hormones and their glucuronides in surface water and waste water in The Netherlands [J].
Belfroid, AC ;
Van der Horst, A ;
Vethaak, AD ;
Schäfer, AJ ;
Rijs, GBJ ;
Wegener, J ;
Cofino, WP .
SCIENCE OF THE TOTAL ENVIRONMENT, 1999, 225 (1-2) :101-108
[3]
Evaluation of two new examples of graphitized carbon blacks for use in solid-phase extraction cartridges [J].
Crescenzi, C ;
DiCorcia, A ;
Passariello, G ;
Samperi, R ;
Carou, MIT .
JOURNAL OF CHROMATOGRAPHY A, 1996, 733 (1-2) :41-55
[4]
Identification of estrogenic chemicals in STW effluent. 1. Chemical fractionation and in vitro biological screening [J].
Desbrow, C ;
Routledge, EJ ;
Brighty, GC ;
Sumpter, JP ;
Waldock, M .
ENVIRONMENTAL SCIENCE & TECHNOLOGY, 1998, 32 (11) :1549-1558
[5]
Structure/activity relationships [J].
Dodge, JA .
PURE AND APPLIED CHEMISTRY, 1998, 70 (09) :1725-1733
[6]
Environmental effects of endocrine disruptors and current methodologies for assessing wildlife health effects [J].
Jimenez, B .
TRAC-TRENDS IN ANALYTICAL CHEMISTRY, 1997, 16 (10) :596-606
[7]
Lee HB, 1998, J AOAC INT, V81, P1209
[8]
Metabolism and fate of xeno-oestrogens in man [J].
Liehr, JG ;
Somasunderam, A ;
Roy, D .
PURE AND APPLIED CHEMISTRY, 1998, 70 (09) :1747-1758
[9]
Novel monitoring strategies for xenoestrogens [J].
Oosterkamp, AJ ;
Hock, B ;
Seifert, M ;
Irth, H .
TRAC-TRENDS IN ANALYTICAL CHEMISTRY, 1997, 16 (10) :544-553
[10]
PARKER GA, 1991, J ASSOC OFF ANA CHEM, V74, P868