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Determination of estrogens and estrogen mimics by solid-phase extraction with liquid chromatography-tandem mass spectrometry
Journal of Chromatography B ( IF 3 ) Pub Date : 2021-01-20 , DOI: 10.1016/j.jchromb.2021.122559
Yejin Li 1 , Linyan Yang 2 , Huajun Zhen 1 , Xueming Chen 3 , Mei Sheng 1 , Kai Li 1 , Weibo Xue 1 , Huihui Zhao 1 , Shujuan Meng 4 , Guomin Cao 2
Affiliation  

An analytical method has been developed and validated for the determination of six estrogens and estrogen mimics, namely estriol (E3), bisphenol A (BPA), 17β-estradiol (E2), estrone (E1), ethynyl estradiol (EE2) and dienestrol (DIE), with frequent occurrence in the natural environment. Solid phase extraction coupled with liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS) using electrospray ionization (ESI) in a negative mode was applied to concentration, identification, and quantification of estrogens and estrogen mimics. The SPE conditions were optimized as the selection of C18 as cartridges and MeOH as an eluent, and the control of solution pH at 9.0. The method was validated by satisfactory recoveries (80–130%) and intra-day and inter-day precision (<18.4%, as relative standard deviation), and excellent linearity for calibration curves (R2 > 0.996). The limits of detection (LODs) for six target estrogenic compounds ranged between 2.5 and 19.2 ng/L. The effects of matrix background on the determination were evaluated in terms of LODs, LOQs, analyte recovery, and slopes of calibration curves in five different water matrices. Matrix effects by tap water were negligible. However, both matrix suppression and enhancement (i.e., E3, E1, DIE) were observed in surface water and wastewater. The positive correlation between LODs and TOC in various water matrices indicated the negative effect of organic pollutants on the method sensitivity. The sum of target estrogenic compounds in environmental samples were within 17–9462 ng/L.



中文翻译:

液相色谱-串联质谱固相萃取法测定雌激素和雌激素模拟物

已开发出一种分析方法,用于确定六种雌激素和雌激素模拟物,即雌三醇(E3),双酚A(BPA),17β-雌二醇(E2),雌酮(E1),乙炔基雌二醇(EE2)和二烯雌酚( DIE),在自然环境中经常发生。固相萃取与液相色谱串联质谱(SPE-LC-MS / MS)结合使用负离子模式的电喷雾电离(ESI)用于雌激素和雌激素模拟物的浓缩,鉴定和定量。通过选择C18作为色谱柱和选择MeOH作为洗脱液以及将溶液的pH控制在9.0,可以优化SPE条件。该方法通过令人满意的回收率(80–130%)以及日内和日间精度(<18.4%,相对标准偏差)进行了验证,R 2  > 0.996)。六个目标雌激素化合物的检出限(LOD)在2.5至19.2 ng / L之间。根据LOD,LOQ,分析物回收率和五个不同水基质中校准曲线的斜率评估了基质背景对测定的影响。自来水对基质的影响可以忽略不计。但是,在地表水和废水中都观察到了基质抑制和增强作用(即E3,E1,DIE)。各种水基质中LOD与TOC之间的正相关关系表明有机污染物对方法灵敏度的负面影响。环境样品中目标雌激素化合物的总量在17–9462 ng / L之内。

更新日期:2021-02-28
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