RESUMO
Endocrine disruptors are a group of organic compounds widely used, which are ubiquitous in the environment and in biological samples. The main effect of these compounds is associated with their ability to mimic or block the action of natural hormones in living organisms, including humans. Parabens (esters of p-hydroxybenzoic acid) belong to this group of compounds. In this work, we propose a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to asses the presence of parabens most commonly used in industrial applications (methyl-, ethyl-, propyl- and butyl-paraben) in samples of human placental tissue. The method involves the extraction of the analytes from the samples using ethyl acetate, followed by a clean-up step using centrifugation prior to their quantification by LC-MS/MS using an atmospheric pressure chemical ionization (APCI) interface in the negative mode. Deuterated bisphenol A (BPA-d(16)) was used as surrogate. Found detection limits (LOD) ranged from 0.03 to 0.06 ng g(-1) and quantification limits (LOQ) from 0.1 to 0.2 ng g(-1), while inter- and intra-day variability was under 13.8%. The method was validated using standard addition calibration and a spike recovery assay. Recovery rates for spiked samples ranged from 82% to 108%. This method was satisfactorily applied for the determination of parabens in 50 placental tissue samples collected from women who live in the province of Granada (Spain).
Assuntos
Cromatografia Líquida/métodos , Parabenos/análise , Placenta/química , Espectrometria de Massas em Tandem/métodos , Feminino , Humanos , Limite de Detecção , Gravidez , Reprodutibilidade dos TestesRESUMO
The group of compounds commonly called endocrine disruptors covers a wide range of synthetic and natural substances able to alter the normal hormone function of wildlife and humans, consequently causing adverse health effects. Bisphenol A (BPA) and its chlorinated derivatives are some of these compounds. In this work, we propose a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to determine these compounds in human placental tissue samples. The method involves an extraction phase of the extracts from the samples using ethyl acetate, followed by a clean-up phase by centrifugation prior to their quantification by LC-MS/MS using an atmospheric pressure chemical ionization (APCI) interface in the negative mode. Deuterated Bisphenol A (BPA-d(16)) was used as internal standard. Found detection limits (DL) ranged from 0.2 to 0.6 ng g(-1) and quantification limits (QL) from 0.5 to 2.0 ng g(-1) for Bisphenol A and its chlorinated derivatives, while inter- and intra-day variability was under 8.1%. The method was validated using standard addition calibration and a spike recovery assay. Recovery rates for spiked samples ranged from 97% to 105%. This method was satisfactorily applied to the determination of BPA and its chlorinated derivatives in 49 placental tissue samples collected from women who live in the province of Granada (Spain).
Assuntos
Compostos Clorados/análise , Cromatografia Líquida/métodos , Hidrocarbonetos Clorados/análise , Fenóis/análise , Placenta/química , Espectrometria de Massas em Tandem/métodos , Compostos Benzidrílicos , Compostos Clorados/química , Disruptores Endócrinos/análise , Disruptores Endócrinos/química , Feminino , Humanos , Hidrocarbonetos Clorados/química , Modelos Lineares , Fenóis/química , Gravidez , Reprodutibilidade dos Testes , Sensibilidade e EspecificidadeRESUMO
Alkylphenols (APs) and AP ethoxylates are environmental contaminants with endocrine disrupting activities in wildlife and humans. They have been largely used in industrial, agricultural, and domestic applications. Despite strong concerns about the consequences of human exposure to endocrine disrupters, little information is available on the presence in humans of compounds such as APs. The aim of the present study was to determine 4-nonylphenol (NP) and 4-octylphenol (OP) residues in adipose tissue of non-occupationally exposed women living in Southern Spain. NP was detected in 100% (n=20/20) and OP in 23.5% (n=4/20) of samples, with median levels of 57 and 4.5 ng g(-1) adipose tissue, respectively. Body mass index emerged as a determinant of exposure since it was associated with NP levels (p=0.041). Adipose tissue NP and OP levels are similar to the few data previously published in other countries. This is the first report on NP and OP levels in a population in Southern Spain. Further research is needed to determine trends in human exposure to these compounds and to investigate their consequences.