Arid
DOI10.1007/s00216-009-3428-y
Development and validation of an analytical method by LC-MS/MS for the quantification of estrogens in sewage sludge
Gabet-Giraud, Virginie1; Miege, Cecile1; Herbreteau, Bernard2; Hernandez-Raquet, Guillermina3; Coquery, Marina1
通讯作者Coquery, Marina
来源期刊ANALYTICAL AND BIOANALYTICAL CHEMISTRY
ISSN1618-2642
EISSN1618-2650
出版年2010
卷号396期号:5页码:1841-1851
英文摘要

A sensitive method for the simultaneous analysis of five estrogens in sewage sludge was developed. The extraction and purification steps were optimized and the matrix effects were evaluated. The chromatographic gradient was optimized to limit matrix effects and the analysis step was performed by LC-MS/MS. The method consists of an ASE(R) extraction with a solvent mixture water/methanol 80/20 nu/nu at 100 degrees C followed by two consecutive purifications on Oasis HLB(R) and florisil cartridges. A thorough validation of the developed method was performed. Recoveries determined at two different spiking levels ranged between 86% and 126% depending on the molecule. Repeatability was evaluated on five replicates of the same sludge sample spiked at two different levels and measuring native estrogens in triplicates of 12 sludge samples. Relative standard deviations obtained a range of between 2% and 27%. Reproducibility was also studied by analyzing the same sludge on four different days: the relative standard deviation ranged between 14% and 20% for E1, beta E2 and E3. For alpha E2, poor reproducibility (68%) was observed but it was linked to the very low quantity of alpha E2 present in the sludge sample and not to the method performance. The specificity of the method was evaluated on various sludge samples spiked at different spiking levels showing that performances of the proposed method were not modified by matrix effects. Finally, sensitivity of the method was evaluated taking into account both instrumental sensitivity and matrices; the estimated limits of quantification were around 1 ng/g for E1, between 2 and 4 ng/g for alpha E2, beta E2, and E3 and around 5 ng/g for EE2.


英文关键词Estrogens LC-MSMS analysis Sewage sludge Matrix effects Wastewater treatment plant Method validation
类型Article
语种英语
国家France
收录类别SCI-E
WOS记录号WOS:000274742900025
WOS关键词TANDEM MASS-SPECTROMETRY ; SOLID-PHASE EXTRACTION ; STEROID SEX-HORMONES ; WASTE-WATER ; LIQUID-CHROMATOGRAPHY ; ENDOCRINE DISRUPTORS ; ENVIRONMENTAL MATRICES ; AQUEOUS MATRICES ; RIVER SEDIMENTS ; PHARMACEUTICALS
WOS类目Biochemical Research Methods ; Chemistry, Analytical
WOS研究方向Biochemistry & Molecular Biology ; Chemistry
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/163153
作者单位1.Cemagref, UR MALY, F-69336 Lyon, France;
2.Univ Lyon, CNRS, UMR5180, Sci Analyt Lab, F-69622 Villeurbanne, France;
3.INRA, UR050, Lab Biotechnol Environm, F-11100 Narbonne, France
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GB/T 7714
Gabet-Giraud, Virginie,Miege, Cecile,Herbreteau, Bernard,et al. Development and validation of an analytical method by LC-MS/MS for the quantification of estrogens in sewage sludge[J],2010,396(5):1841-1851.
APA Gabet-Giraud, Virginie,Miege, Cecile,Herbreteau, Bernard,Hernandez-Raquet, Guillermina,&Coquery, Marina.(2010).Development and validation of an analytical method by LC-MS/MS for the quantification of estrogens in sewage sludge.ANALYTICAL AND BIOANALYTICAL CHEMISTRY,396(5),1841-1851.
MLA Gabet-Giraud, Virginie,et al."Development and validation of an analytical method by LC-MS/MS for the quantification of estrogens in sewage sludge".ANALYTICAL AND BIOANALYTICAL CHEMISTRY 396.5(2010):1841-1851.
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