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1.
Drug Test Anal ; 8(7): 730-7, 2016 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-26041114

RESUMO

The purpose of this study was to develop a simple, direct, multiresidue highly specific procedure to evaluate the possible surface contamination of selected antineoplastic drugs in several hospital environment sites by using wipe test sampling. 5-fluorouracil (5-FU), carboplatin (C-Pt), cyclophosphamide (CYC), cytarabine (CYT), doxorubicin (DOX), gemcitabine (GEM), ifosfamide (IFO), methotrexate (MET), and mitomycin C (MIT) belong to very different chemical classes but show good ionization properties under electrospray ionization (ESI) conditions (negative ion mode for 5-FU and positive ion mode in all other cases). HPLC (high performance liquid chromatography) coupled with HRMS (high resolution mass spectrometry) appears to be the best technique for direct analysis of these analytes, because neither derivatization nor complex extraction procedure for polar compounds in samples is requested prior the analysis. Sample preparation was limited to washing wipes with appropriate solvents. Chromatographic separation was achieved on C18 reversed phase columns. The HPLC-HRMS/MS method was validated in order to obtain robustness, sensitivity and selectivity. LLOQ (lower limit of quantitation) values provided a sensitivity good enough to evidence the presence of the drugs in a very low concentration range (<1 pg/cm(2) ). The method was applied for a study of real wipe tests coming from many areas from a hospital showing some positive samples. The low quantitation limits and the high specificity due to the high resolution approach of the developed method allowed an accurate description of the working environment that can be used to define procedural rules to limit working place contamination to a minimum. Copyright © 2015 John Wiley & Sons, Ltd.


Assuntos
Antineoplásicos/análise , Cromatografia Líquida de Alta Pressão/métodos , Poluentes Ambientais/análise , Exposição Ocupacional/análise , Espectrometria de Massas em Tandem/métodos , Cromatografia de Fase Reversa/métodos , Hospitais , Humanos , Limite de Detecção
2.
J Chromatogr A ; 1412: 59-66, 2015 Sep 18.
Artigo em Inglês | MEDLINE | ID: mdl-26283533

RESUMO

The analysis of lipid molecules in living organism is an important step in deciphering metabolic pathways. Recently, the zebrafish has been adopted as a valuable animal model system to perform in vivo metabolomics studies, however limited methodologies and protocols are currently available to investigate zebrafish lipidome and even fewer to analyze specific classes of lipids. Here we present an HPLC-HRMS based method to rapidly measure multiple prenol lipid molecules from zebrafish tissues. In particular, we have optimized our method for concurrent detection of ubiquinones (Coenzyme Q6, Coenzyme Q9, Coenzyme Q10), cholesterol, vitamin E (α-tocopherol), vitamin K1 and vitamin K2. The purpose of this study was to compare different ionization modes, mobile phases and stationary phases in order to optimize lipid molecules separation. After HPLC-HRMS parameters selection, several extraction conditions from zebrafish embryos were evaluated. We assessed our methodology by quantitation of analytical recovery on zebrafish extracts from wild-type or zebrafish mutants (barolo) affected by impaired biosynthesis of ubiquinones.


Assuntos
Pentanóis/análise , Peixe-Zebra/metabolismo , Animais , Colesterol/análise , Cromatografia Líquida de Alta Pressão/métodos , Embrião não Mamífero/metabolismo , Hemiterpenos , Espectrometria de Massas/métodos , Mutação , Ubiquinona/análise , Vitamina E/análise , Vitamina K 1/análise , Vitamina K 2/análise , Peixe-Zebra/genética , alfa-Tocoferol/análise
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