Knowledge Resource Center for Ecological Environment in Arid Area
DOI | 10.1007/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
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ISSN | 1618-2642 |
EISSN | 1618-2650 |
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 |
推荐引用方式 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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