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1.
Toxicon ; 174: 1-7, 2020 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-31786272

RESUMO

In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was originally developed for simultaneously quantitative analysis of twelve paralytic shellfish poisoning toxins, referring to STX, NEO, dcSTX, GTX1, GTX2, GTX3, GTX4, GTX5, C1, C2, dcGTX2, and dcGTX3 in bivalve molluscs. Chromatographic separations were performed on a TSK-Gel Amide-80 column (5 µm, 2.0 × 150 mm, Tosoh Corporation) by gradient elution with 2 mmol L-1 ammonium formate solution-acetonitrile (containing 0.1% formic acid) as mobile phases. The samples were pretreated by extraction with acetonitrile-water (80:20, v/v; containing 0.1% formic acid), followed by cleaning up using an Oasis HLB extraction cartridge (500 mg/6 mL). The present method showed good linearity (r2 > 0.99) with the limits of detection (LODs) and limits of quantification (LOQs) ranged from 1.03 to 10.65 µg/kg and 3.43-35.46 µg/kg, respectively for these toxins. Owing to its sensitivity and rapid properties, the presented method was applied to the determination of PSP toxins in bivalve molluscs involved in a food poisoning incident occurred in Zhangzhou, China, in June 2017.


Assuntos
Bivalves/fisiologia , Toxinas Marinhas/análise , Intoxicação por Frutos do Mar , Animais , China , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Limite de Detecção , Frutos do Mar , Extração em Fase Sólida , Espectrometria de Massas em Tandem
2.
Anal Chim Acta ; 767: 50-8, 2013 Mar 12.
Artigo em Inglês | MEDLINE | ID: mdl-23452786

RESUMO

A novel electrochemical DNA biosensor based on graphene-three dimensional nanostructure gold nanocomposite modified glassy carbon electrode (G-3D Au/GCE) was fabricated for detection of survivin gene which was correlated with osteosarcoma. The G-3D Au film was prepared with one-step electrochemical coreduction with graphite oxide and HAuCl4 at cathodic potentials. The active surface area of G-3D Au/GCE was 2.629cm(2), which was about 3.8 times compared to that of a Au-coated GCE under the same experimental conditions, and 8.8 times compared to a planar gold electrode with a similar geometric area. The resultant nanocomposites with high conductivity, electrocatalysis and biocompatibility were characterized by scanning electron microscopy (SEM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). A "sandwich-type" detection strategy was employed in this electrochemical DNA biosensor and the response of this DNA biosensor was measured by CV and amperometric current-time curve detection. Under optimum conditions, there was a good linear relationship between the current signal and the logarithmic function of complementary DNA concentration in a range of 50-5000fM with a detection limit of 3.4fM. This new biosensor exhibited a fast amperometric response, high sensitivity and selectivity and has been used in a polymerase chain reaction assay of real-life sample with a satisfactory result.


Assuntos
Técnicas Biossensoriais , DNA/análise , Técnicas Eletroquímicas , Ouro/química , Grafite/química , Nanopartículas Metálicas/química , Osteossarcoma/genética , Eletrodos , Microscopia Eletrônica de Varredura , Oxirredução , Óxidos/química
3.
Toxicon ; 51(5): 774-9, 2008 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-18222512

RESUMO

Tetrodotoxin (TTX) has been usually analyzed in marine and other sources by HPLC separation, followed by alkaline treatment and fluorescence assay. However, the applications of such methods were limited because of their tedious extraction and derivation procedures. A simpler, rapid LC-MS method, using selected ion-monitoring, has now been developed, and used to identify and quantitate TTX in a marine gastropod of the genus Nassarius, collected from Fijian province of China. The toxin was confirmed comparable to authentic TTX by MS and MSn. In addition, a moderate amount of TTX was detected in the Nassarius by this novel approach, suggesting that Nassarius would be a potential food poison source.


Assuntos
Gastrópodes/química , Tetrodotoxina/análise , Animais , Bioensaio , Cromatografia Líquida/métodos , Gastrópodes/metabolismo , Espectrometria de Massas/métodos , Camundongos , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Tetrodotoxina/metabolismo
4.
Chem Pharm Bull (Tokyo) ; 54(5): 687-9, 2006 May.
Artigo em Inglês | MEDLINE | ID: mdl-16651767

RESUMO

When used as a dietary supplement to achieve and maintain healthy cholesterol levels,Chinese red yeast rice has significant potential to reduce health care costs and contribute to public health by reducing heart disease risk in individuals with moderate elevations of circulating cholesterol levels. Red yeast rice is typical product in Mingbei area of Fujian province. Nine products from different area were measured, using high-performance chromatography (HPLC) with photodiode array detector (PDA) and tandem mass spectrometry (MS) and the results show that the contents of monacolin K in these products were considerably different, and more than the other product.


Assuntos
Produtos Biológicos/química , Lovastatina/análise , Monascus/química , Cromatografia Líquida de Alta Pressão , Indicadores e Reagentes , Espectrometria de Massas , Padrões de Referência , Espectrofotometria Ultravioleta
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