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1.
Anal Bioanal Chem ; 416(2): 449-459, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-37987769

RESUMO

In this work, a complete study of the distribution of emerging mycotoxins in the human body has been carried out. Specifically, the presence of enniatins (A, A1, B, B1) and beauvericin has been monitored in brain, lung, kidney, fat, liver, and heart samples. A unique methodology based on solid-liquid extraction (SLE) followed by dispersive liquid-liquid microextraction (DLLME) was proposed for the six different matrices. Mycotoxin isolation was performed by adding ultrapure water, acetonitrile, and sodium chloride to the tissue sample for SLE, while the DLLME step was performed using chloroform as extraction solvent. Subsequently, the analysis was carried out by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The proposed method allowed limits of quantification (LOQs) to be obtained in a range of 0.001-0.150 ng g-1, depending on the tissue and mycotoxin. The precision was investigated intraday and interday, not exceeding of 9.8% of relative standard deviation. In addition, trueness studies achieved 75 to 115% at a mycotoxin concentration of 25 ng g-1 and from 82 to 118% at 5 ng g-1. The application of this methodology to 26 forensic autopsies demonstrated the bioaccumulation of emerging mycotoxins in the human body since all mycotoxins were detected in tissues. Enniatin B (ENNB) showed a high occurrence, being detected in 100% of liver (7 ± 13 ng g-1) and fat samples (0.2 ± 0.8 ng g-1). The lung had a high incidence of all emerging mycotoxins at low concentrations, while ENNB, ENNB1, and ENNA1 were not quantifiable in heart samples. Co-occurrence of mycotoxins was also investigated, and statistical tests were applied to evaluate the distribution of these mycotoxins in the human body.


Assuntos
Microextração em Fase Líquida , Micotoxinas , Humanos , Espectrometria de Massa com Cromatografia Líquida , Espectrometria de Massas em Tandem/métodos , Micotoxinas/análise , Cromatografia Líquida de Alta Pressão
2.
Molecules ; 28(11)2023 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-37298771

RESUMO

The botanical origin of honey determines its composition and hence properties and product quality. As a highly valued food product worldwide, assurance of the authenticity of honey is required to prevent potential fraud. In this work, the characterisation of Spanish honeys from 11 different botanical origins was carried out by headspace gas chromatography coupled with mass spectrometry (HS-GC-MS). A total of 27 volatile compounds were monitored, including aldehydes, alcohols, ketones, carboxylic acids, esters and monoterpenes. Samples were grouped into five categories of botanical origins: rosemary, orange blossom, albaida, thousand flower and "others" (the remaining origins studied, due to the limitation of samples available). Method validation was performed based on linearity and limits of detection and quantification, allowing the quantification of 21 compounds in the different honeys studied. Furthermore, an orthogonal partial least squares-discriminant analysis (OPLS-DA) chemometric model allowed the classification of honey into the five established categories, achieving a 100% and 91.67% classification and validation success rate, respectively. The application of the proposed methodology was tested by analysing 16 honey samples of unknown floral origin, classifying 4 as orange blossom, 4 as thousand flower and 8 as belonging to other botanical origins.


Assuntos
Mel , Compostos Orgânicos Voláteis , Cromatografia Gasosa-Espectrometria de Massas/métodos , Mel/análise , Compostos Orgânicos Voláteis/análise , Análise Discriminante , Flores/química
3.
Foods ; 10(2)2021 Feb 03.
Artigo em Inglês | MEDLINE | ID: mdl-33546285

RESUMO

After the International Agency for Research on Cancer (IARC) classified ingested nitrites and nitrates as "probably carcinogenic to humans" under conditions favoring endogenous nitrosation, several meat products labeled as "made without nitrite" were launched. In order to distinguish uncured products truly made without nitrite from cured products made with any nitrite source (vegetal or mineral), this article presents an approach to detect and quantify nitrite from different origins added to meat. The method consists on the determination of nitrous oxide as a target compound using headspace gas chromatography-mass spectrometry (HS-GC-MS). Nitrous oxide (N2O) is formed after two reduction steps: from nitrite to nitric oxide (NO) and then to N2O. The NO is bound to myoglobin (Mb) or metmyoglobin (Met-Mb), forming a complex, which is subsequently released using sulfuric acid, which also favors the reduction to N2O. The HS-GC-MS conditions were split ratio 1:10; injection temperature at 70 °C; incubation temperature at 30 °C and time 45 min; and injection volume 1 mL. As a result, a relationship was established between the concentration of nitrite in cooked ham samples and the area of the N2O peak generated, meaning that this method allows the quantification of added nitrite within a concentration range of 10 to 100 mg kg-1.

4.
Talanta ; 205: 120123, 2019 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-31450393

RESUMO

The recognized properties of honey together with its price have, almost inevitably, led to economically motivated adulteration. In this work, headspace gas chromatography coupled to ion mobility spectrometry (HS-GC-IMS) is proposed for the differentiation of honey according to its purity and the level of adulteration by sugar cane or corn syrups. An easy and rapid sample treatment, consisting of incubating 1 g of honey at 100 °C for 15 min and then injecting 750 µL of the sample headspace into the GC-IMS system, is proposed. A 3-dimensional data map is obtained in 32 min. The proposed method was used for the analysis of 198 honey samples (56 pure honeys of different botanical origins, 71 honeys adulterated with sugar cane syrup and 71 adulterated with corn syrup). The influence of the adulterant on variations in the honey sample spectrum was studied. In order to obtain chemometric models for the detection of adulterated honey samples, the data obtained by HS-GC-IMS were processed selecting the significant markers of the spectrum fingerprint. OPLS-DA models were constructed using 80% of the samples, and the remaining 20% were used for method validation. The differentiation between pure and adulterated honeys had a validation success of 97.4%, and the assessment of adulterant content was obtained with a 93.8% validation success rate for both adulterant agents assayed. Nine commercial honey samples were analysed using the proposed methodology, and seven of them were classified as adulterated.


Assuntos
Contaminação de Alimentos/análise , Mel/análise , Cromatografia Gasosa/métodos , Xarope de Milho Rico em Frutose/análise , Espectrometria de Mobilidade Iônica/métodos
5.
Rev Enferm ; 30(6): 9-12, 2007 Jun.
Artigo em Espanhol | MEDLINE | ID: mdl-17685139

RESUMO

The authors describe the school children health activities developed by the Primary Health Care Area 1 in Madrid Teams from the 1996-97 academic year until the 2004-05 year During this time period, 559 EPS activities were carried out, 56% belonged to the Program to Promote Health in School in Area 1. The other 44% are projects developed by sanitary professionals. These activities were developed in 70 educational centers, focusing on different groups: 91% on students, 6% on parents and 3% on teachers. This analysis demonstrates the leadership of nursing professionals have in the EPS school program. These activities worked mainly with students.


Assuntos
Educação em Saúde , Papel do Profissional de Enfermagem , Enfermeiras e Enfermeiros , Ensino , Criança , Humanos
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