scholarly journals Methods for simultaneous determination of legacy and insensitive munition (IM) constituents in aqueous, soil/sediment, and tissue matrices

2021 ◽  
Author(s):  
Rebecca Crouch ◽  
Jared Smith ◽  
Bobbi Stromer ◽  
Christian Hubley ◽  
Samuel Beal ◽  
...  
Keyword(s):  
Environmental Protection Agency ◽  
High Performance ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Primary Objective ◽  
Environmental Matrices ◽  
Tissue Extracts ◽  
Soil Sediment ◽  
Analytical Separation

Currently, no standard method exists for analyzing insensitive munition (IM) compounds in environmental matrices, with or without concurrent legacy munition compounds, resulting in potentially inaccurate determinations. The primary objective of this work was to develop new methods of extraction, pre-concentration, and analytical separation/quantitation of 17 legacy munition compounds along with several additional IM compounds, IM breakdown products, and other munition compounds that are not currently included in U.S. Environmental Protection Agency (EPA) Method 8330B. Analytical methods were developed to enable sensitive, simultaneous detection and quantitation of the 24 IM and legacy compounds, including two orthogonal high-performance liquid chromatography (HPLC) column separations with either ultraviolet (UV) or mass spectrometric (MS) detection. Procedures were developed for simultaneous extraction of all 24 analytes and two surrogates (1,2-dinitrobenzene, 1,2-DNB; o-NBA) from high- and low-level aqueous matrices and solid matrices, using acidification, solid phase extraction (SPE), or solvent extraction (SE), respectively. The majority of compounds were recovered from four tissue types within current limits for solids, with generally low recovery only for Tetryl (from 4 to 62%). A preparatory chromatographic interference removal procedure was adapted for tissue extracts, as various analytical interferences were observed for all studied tissue types.

scholarly journals DETERMINATION OF SULFONAMIDES IN CHICKEN MEAT BY SOLID PHASE EXTRACTION AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

1970 ◽  
Vol 63 ◽  
Author(s):  
C. T. Matea ◽  
C. Bele ◽  
F. Dulf
Keyword(s):  
High Performance ◽  
Ammonium Acetate ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Gradient Elution ◽  
Normal Phase ◽  
Chicken Meat ◽  
Liquid Liquid Extraction ◽  
Halogenated Solvents

This paper describes a method for the simultaneous detection and quantification of six sul-fonamides in chicken meat using normal phase cartridge clean-up and HPLC with UV detection . A liquid – liquid extraction and Sep- Pak silica clean-up procedure which minimizes the presence of halogenated solvents was used for sample preparation . The HPLC determination was performed using a RP C 18 column and sulfonamides were detected at 266 nm. Mobile phase was 0.01 M ammonium acetate pH 4.6 ( A ) and methanol ( B). Chromatographic separation was obtained by gradient elution ( 22 % B to 50 % within 17 min , back to 22 % in 2 min, equilibration for 5 min).Average recoveries of analytes from spiked meat were higher than 74 % .

scholarly journals Optimization of a Method for Extraction and Determination of Residues of Selected Antimicrobials in Soil and Plant Samples Using HPLC-UV-MS/MS

2021 ◽  
Vol 18 (3) ◽  
pp. 1159
Author(s):  
Klaudia Kokoszka ◽  
Agnieszka Kobus ◽  
Sylwia Bajkacz
Keyword(s):  
Nalidixic Acid ◽  
High Performance ◽  
Solid Phase ◽  
Sewage Treatment ◽  
Animal Manure ◽  
Uv Detector ◽  
Citrate Buffer ◽  
High Biological Activity ◽  
Extraction Solvent

The residues of antimicrobials used in human and veterinary medicine are popular pollutants of anthropogenic origin. The main sources of introducing antimicrobials into the environment are sewage treatment plants and the agricultural industry. Antimicrobials in animal manure contaminate the surrounding soil as well as groundwater, and can be absorbed by plants. The presence of antimicrobials in food of plant origin may pose a threat to human health due to their high biological activity. As part of the research, a procedure was developed for the extraction and determination of ciprofloxacin, enrofloxacin, cefuroxime, nalidixic acid and metronidazole in environmental samples (soil and parsley root). An optimized solid-liquid extraction (SLE) method was used to separate antimicrobials from the solid samples and a mixture of citrate buffer (pH = 4): methanol (1:1; v/v) was used as the extraction solvent. Solid phase extraction (SPE) with OASIS® HLB cartridges was used to purify and pre-concentrate the sample. The recovery of the developed method was in the range of 55–108%. Analytes were determined by high-performance liquid chromatography coupled with an ultraviolet (UV) detector and a tandem mass spectrometer (HPLC-UV-MS/MS). The procedure was validated and applied to the determination of selected antimicrobials in soil and parsley root samples. Five types of soil and five types of parsley roots of different origins were analyzed. The presence of nalidixic acid in the parsley root samples was found in the concentration range of 0.14–0.72 ng g−1. It has been shown that antimicrobials are absorbed by the plant and can accumulate antimicrobials in its edible parts.

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