scholarly journals Preparative, extraction, and analytical methods for simultaneous determination of legacy and insensitive munition (IM) constituents in aqueous, soil or sediment, and tissue matrices

2021 ◽  
Author(s):  
Rebecca Crouch ◽  
Jared Smith ◽  
Bobbi Stromer ◽  
Christian Hubley ◽  
Samuel Beal ◽  
...  
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Direct Injection ◽  
Treatment Method ◽  
Extraction Methods ◽  
Environmental Matrices ◽  
Long Term Effects ◽  
Tissue Samples ◽  
New Methods ◽  
Supply Costs

No standard method exists for determining levels of insensitive munition (IM) compounds in environmental matrices. This project resulted in new methods of extraction, analytical separation and quantitation of 17 legacy and 7 IM compounds, daughter products of IM, and other munition compounds absent from USEPA Method 8330B. Extraction methods were developed for aqueous (direct-injection and solid-phase extraction [SPE]), soil, sediment, and tissue samples using laboratory-spiked samples. Aqueous methods were tested on 5 water sources, with 23 of 24 compounds recovered within DoD QSM Ver5.2 limits. New solvent extraction (SE) methods enabled recovery of all 24 compounds from 6 soils within QSM limits, and a majority of the 24 compounds were recovered at acceptable levels from 4 tissues types. A modified chromatographic treatment method removed analytical interferences from tissue extracts. Two orthogonal high-performance liquid chromatography-ultraviolet (HPLC-UV) separation methods, along with an HPLC–mass spectrometric (HPLC-MS) method, were developed. Implementing these new methods should reduce labor and supply costs by approximately 50%, requiring a single extraction and sample preparation, and 2 analyses rather than 4. These new methods will support environmental monitoring of IM and facilitate execution of risk-related studies to determine long-term effects of IM compounds.

Methods for simultaneous determination of 29 legacy and insensitive munition (IM) constituents in aqueous, soil-sediment, and tissue matrices by high-performance liquid chromatography (HPLC)

2021 ◽  
Author(s):  
Bobbi Stromer ◽  
Rebecca Crouch ◽  
Katrinka Wayne ◽  
Ashley Kimble ◽  
Jared Smith ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solvent Extraction ◽  
Environmental Protection Agency ◽  
High Performance ◽  
Solid Phase ◽  
Degradation Products ◽  
Direct Injection ◽  
High Water ◽  
Hplc Method

Standard methods are in place for analysis of 17 legacy munitions compounds and one surrogate in water and soil matrices; however, several insensitive munition (IM) and degradation products are not part of these analytical procedures. This lack could lead to inaccurate determinations of munitions in environmental samples by either not measuring for IM compounds or using methods not designed for IM and other legacy compounds. This work seeks to continue expanding the list of target analytes currently included in the US Environmental Protection Agency (EPA) Method 8330B. This technical report presents three methods capable of detecting 29 legacy, IM, and degradation products in a single High Performance Liquid Chromatography (HPLC) method with either ultraviolet (UV)-visible absorbance detection or mass spectrometric detection. Procedures were developed from previously published works and include the addition of hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX); hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX); hexahydro-1,3,5-trinitroso-1,3,5-triazine (TNX); 2,4-diamino-6-nitrotoluene (2,4-DANT); and 2,6-diamino-4-nitrotoluene (2,6-DANT). One primary analytical method and two secondary (confirmation) methods were developed capable of detecting 29 analytes and two surrogates. Methods for high water concentrations (direct injection), low-level water concentrations (solid phase extraction), soil (solvent extraction), and tissue (solvent extraction) were tested for analyte recovery of the new compounds.

scholarly journals COMPARISON OF THREE EXTRACTION METHODS OF ALLOPURINOL IN URIC ACID HERBAL MEDICINE WITH HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY QUANTIFICATION

2021 ◽  
pp. 141-147
Author(s):  
RIMADANI PRATIWI ◽  
RASPATI D. MULYANINGSIH ◽  
NYI M. SAPTARINI
Keyword(s):  
Herbal Medicine ◽  
High Performance ◽  
Solid Phase ◽  
Extraction Methods ◽  
Liquid Extraction ◽  
Filtering Method ◽  
Liquid Liquid Extraction ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Parameters Of Accuracy

Objective: This study was aimed to understand and determine the effectiveness of allopurinol extraction in herbal medicine from three extraction methods based on parameters of accuracy and precision. Methods: The study consisted of three methods including dissolving and filtering, liquid-liquid extraction, and solid-phase extraction with mixed-mode cation exchanger (SPE-MCX). The procedures were carried out using NaOH and HCl in dissolving and filtering method; methanol, HCl, and ethyl acetate in liquid-liquid extraction; and NH4OH elution solvent in SPE-MCX. Results: The results showed that extraction effectiveness based on accuracy level was the dissolving and filtering method>SPE-MCX>liquid-liquid extraction with % recovery+SD of 91.314+2.903%, 87.533+4.950%, and 54.549+3.517%, respectively. The precision level was the dissolution and filtering method>SPE-MCX>liquid-liquid extraction based on % relative standard deviations (RSD) of 3.18%, 5.226%, and 6.446%, respectively. Conclusion: It can be concluded that the allopurinol extraction method with the highest effectiveness based on accuracy and precision parameters in herbal medicine is the dissolving and filtering method.

scholarly journals A Review of the Analytical Methods for the Determination of 4(5)-Methylimidazole in Food Matrices

Chemosensors ◽  
2021 ◽  
Vol 9 (11) ◽  
pp. 322
Author(s):  
Panagiota-Kyriaki Revelou ◽  
Marinos Xagoraris ◽  
Eleftherios Alissandrakis ◽  
Christos S. Pappas ◽  
Petros A. Tarantilis
Keyword(s):  
Mass Spectrometry ◽  
Analytical Methods ◽  
High Performance ◽  
Water Solubility ◽  
Solid Phase ◽  
Sample Pretreatment ◽  
Extraction Methods ◽  
Exchange Chromatography ◽  
Food Matrices

4(5)-Methylimidazole (4(5)MEI) is a product of the Maillard reaction between sugars and amino acids, which occurs during the thermal processing of foods. This compound is also found in foods with caramel colorants additives. Due to its prevalence in foods and beverages and its potent carcinogenicity, 4(5)MEI has received federal and state regulatory agency attention. The aim of this review is to present the extraction procedures of 4(5)MEI from food matrices and the analytical methods for its determination. Liquid and gas chromatography coupled with mass spectrometry are the techniques most commonly employed to detect 4(5)MEI in food matrices. However, the analysis of 4(5)MEI is challenging due to the high polarity, water solubility, and the absence of chromophores. To overcome this, specialized sample pretreatment and extraction methods have been developed, such as solid-phase extraction and derivatization procedures, increasing the cost and the preparation time of samples. Other analytical methods for the determination of 4(5)MEI, include capillary electrophoresis, paper spray mass spectrometry, micellar electrokinetic chromatography, high-performance cation exchange chromatography, fluorescence-based immunochromatographic assay, and a fluorescent probe.

scholarly journals An Analytical Method to Screen for Six Thyreostatic Drug Residues in the Thyroid Gland andMuscle Tissues of Food Producing Animals by Liquid Chromatography with Ultraviolet Absorption Detection and Liquid Chromatography/Mass Spectrometry

2006 ◽  
Vol 89 (2) ◽  
pp. 567-575 ◽  
Author(s):  
Philip E Asea ◽  
James D MacNeil ◽  
Joe O Boison
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Thyroid Tissue ◽  
Internal Standard ◽  
Gradient Elution ◽  
Internal Standards ◽  
Tissue Samples ◽  
Muscle Tissues

Abstract A method was developed and validated to screen for residues of the thyreostatic drugs, tapazole (TAP), mercaptobenzimidazole (MBI), thiouracil (TU), methylthiouracil (MTU), propylthiouracil (PrTU), and phenylthiouracil (PhTU) in bovine, equine, ovine, and porcine thyroid and muscle tissues at concentrations 5 ng/g using 2-methoxy-mercaptobenzimidazole (MeMBI) and dimethylthiouracil (DMTU) as internal standards. In this method, the drugs were solvent extracted from thyroid and muscle tissue and cleaned up on an amino-propyl solid-phase extraction (SPE) cartridge. The unretained fraction containing TAP and MBI and the internal standard, MeMBI, was collected as Fraction 1. The retained fraction containing TU, MTU, PrTU, PhTU, and the internal standard, DMTU, was eluted with 3 acetic acidisopropanol as Fraction 2. Fraction 1 was further cleaned up on an alumina B SPE cartridge and analyzed by gradient elution on a C18 high-performance liquid chromatography (HPLC) column with ultraviolet detection at wavelengths of 255 and 300 nm. Fraction 2 was taken to dryness, derivatized with 4-chloro-7-nitrobenzo-2-furazan at pH 8, and analyzed by gradient elution on a C18 LC column with mass spectrometry (MS) detection. Any presumptive positive test results were submitted for further analysis by LC/MS/MS. The validated method was applied to the analysis of over 300 thyroid tissue samples.

scholarly journals Detecção de Resíduos de Agrotóxicos no Mel de Abelha

2014 ◽  
Vol 2 (2) ◽  
pp. 17
Author(s):  
F. M. Silva ◽  
D. C. Coelho ◽  
A. V. Machado ◽  
R. O. Costa
Keyword(s):  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Pesticide Residues ◽  
High Performance ◽  
Solid Phase ◽  
Foreign Market ◽  
Extraction Methods ◽  
Uv Detector ◽  
Residue Detection ◽  
The Matrix

<p>As abelhas A. melífera são uns dos mais importantes polinizadores de culturas, além disso, elas produzem mel, própolis, geleia real e cera. O mel, principal produto da atividade apícola, utilizado como alimento, adoçante e para fins terapêuticos (apiterapia), tem a imagem de ser natural, saudável e limpo sendo esse um produto muito valorizado no mercado externo por isso, a busca por rigorosos padrões de qualidade se torna necessária para atender a um mercado consumidor cada vez mais exigente. Dessa forma a identificação da origem floral e geográfica, a ocorrência de adulterações e as contaminações, principalmente com antibióticos e agrotóxicos no mel tem se tornado uma rota importante devido os quais podem acarretar problemas de saúde ao consumidor. A dispersão da matriz em fase sólida (MSPD) combinada às técnicas cromatográficas modernas como cromatografia a gás (GC) e cromatografia a líquido (HPLC) é uma alternativa para evitar os diversos inconvenientes encontrados nos métodos clássicos de extração. A proposta desse trabalho foi pesquisar os diferentes tipos de Análises e metodologias de detecção de resíduos de agrotóxicos no mel de abelha Apresentando diferentes metodologias para a execução de estudos para validação de metodologia em métodos analítico, utilizando as técnicas de dispersão da matriz em fase sólida, cromatografia a gás acoplada à espectrometria de massas e cromatografia líquida de alta eficiência com detector espectrofotométrico com arranjo de diodos.</p><p><strong>Pesticide Residues in Honey Pesticide Residues detection in Bee honey</strong></p><pre> </pre><p><strong> </strong>A. mellifera bees are one of the most important pollinators of crops in addition they produce honey, propolis, royal jelly and wax. Honey, the main product of beekeeping, used as food, sweetener and in therapy (apitherapy), has the image of being natural, healthy and clean making a highly valued product in the foreign market so the search for rigorous standards of quality is needed to meet a consumer market increasingly demanding. Thus the identification of floral and geographical origin, the occurrence of tampering and contamination, especially with antibiotics and pesticides in honey has become an important route because which can cause health problems to consumers. The dispersion of the solid phase matrix (PDDM) combined with modern chromatographic techniques as gas chromatography (GC) and liquid chromatography (HPLC) is an alternative to avoid the various drawbacks found in classical extraction methods. The purpose of this study was to investigate the different types of analyzes and pesticide residue detection methodologies in honey Introducing different methodologies for carrying out studies for validation of a method in analytical methods, using the matrix dispersion techniques in solid phase, gas chromatography coupled to mass spectrometry and high-performance liquid chromatography with UV detector with diode array.</p>

scholarly journals Metabolite Profiling of Meridianin C In Vivo of Rat by UHPLC/Q-TOF MS

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Guozhe Zhang ◽  
Linxia Xiao ◽  
Liang Qi
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Solid Phase ◽  
Extraction Methods ◽  
Mass Spectral Fragmentation ◽  
Mass Spectral ◽  
Flight Mass Spectrometry ◽  
Fragmentation Patterns ◽  
Tof Ms

Meridianin C (MC), as a marine alkaloid, is a potent protein kinase inhibitor which exhibits good anticancer activity. However, the in vivo metabolism of MC has not been described to date. In this study, an ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF MS) method is employed to investigate the in vivo metabolites of MC in rats. Plasma, bile, urine, and feces are collected after a single oral dose of MC. Protein precipitation, solid phase extraction (SPE), and ultrasonic extraction methods are used to prepare samples. Based on the mass spectral fragmentation patterns, elution order, and retrieving literatures, a total of 13 metabolites of MC were detected and tentatively identified, utilizing MetaboLynx software. The metabolic pathways of MC in rats include N- or O-glucuronidation, O-sulfation, N-hydroxylation, dihydroxylation, and trihydroxylation. The relative content of the metabolites in each kinds of biological samples is also evaluated. This study will help to understand the in vivo properties of MC for the future usage.

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