scholarly journals Application of Bar Adsorptive Microextraction for the Determination of Levels of Tricyclic Antidepressants in Urine Samples

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3101
Author(s):  
Mariana N. Oliveira ◽  
Oriana C. Gonçalves ◽  
Samir M. Ahmad ◽  
Jaderson K. Schneider ◽  
Laiza C. Krause ◽  
...  
Keyword(s):  
Tricyclic Antidepressants ◽  
Matrix Effects ◽  
Activated Carbons ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Experimental Conditions ◽  
Analytical Methodology ◽  
Low Efficiency

This work entailed the development, optimization, validation, and application of a novel analytical approach, using the bar adsorptive microextraction technique (BAμE), for the determination of the six most common tricyclic antidepressants (TCAs; amitriptyline, mianserin, trimipramine, imipramine, mirtazapine and dosulepin) in urine matrices. To achieve this goal, we employed, for the first time, new generation microextraction devices coated with convenient sorbent phases, polymers and novel activated carbons prepared from biomaterial waste, in combination with large-volume-injection gas chromatography-mass spectrometry operating in selected-ion monitoring mode (LVI-GC-MS(SIM)). Preliminary assays on sorbent coatings, showed that the polymeric phases present a much more effective performance, as the tested biosorbents exhibited low efficiency for application in microextraction techniques. By using BAμE coated with C18 polymer, under optimized experimental conditions, the detection limits achieved for the six TCAs ranged from 0.2 to 1.6 μg L−1 and, weighted linear regressions resulted in remarkable linearity (r2 > 0.9960) between 10.0 and 1000.0 μg L−1. The developed analytical methodology (BAμE(C18)/LVI-GC-MS(SIM)) provided suitable matrix effects (90.2–112.9%, RSD ≤ 13.9%), high recovery yields (92.3–111.5%, RSD ≤ 12.3%) and a remarkable overall process efficiency (ranging from 84.9% to 124.3%, RSD ≤ 13.9%). The developed and validated methodology was successfully applied for screening the six TCAs in real urine matrices. The proposed analytical methodology proved to be an eco-user-friendly approach to monitor trace levels of TCAs in complex urine matrices and an outstanding analytical alternative in comparison with other microextraction-based techniques.

scholarly journals A Fast and Validated High Throughput Bar Adsorptive Microextraction (HT-BAµE) Method for the Determination of Ketamine and Norketamine in Urine Samples

Molecules ◽  
2020 ◽  
Vol 25 (6) ◽  
pp. 1438 ◽  
Author(s):  
Samir M. Ahmad ◽  
Mariana N. Oliveira ◽  
Nuno R. Neng ◽  
J.M.F. Nogueira
Keyword(s):  
High Throughput ◽  
Aqueous Media ◽  
Cost Effective ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Large Volume Injection ◽  
Experimental Conditions ◽  
Assay Time

We developed, optimized and validated a fast analytical cycle using high throughput bar adsorptive microextraction and microliquid desorption (HT-BAμE-μLD) for the extraction and desorption of ketamine and norketamine in up to 100 urine samples simultaneously, resulting in an assay time of only 0.45 min/sample. The identification and quantification were carried out using large volume injection-gas chromatography-mass spectrometry operating in the selected ion monitoring mode (LVI-GC-MS(SIM)). Several parameters that could influencing HT-BAµE were assayed and optimized in order to maximize the recovery yields of ketamine and norketamine from aqueous media. These included sorbent selectivity, desorption solvent and time, as well as shaking rate, microextraction time, matrix pH, ionic strength and polarity. Under optimized experimental conditions, suitable sensitivity (1.0 μg L−1), accuracy (85.5–112.1%), precision (≤15%) and recovery yields (84.9–105.0%) were achieved. Compared to existing methods, the herein described analytical cycle is much faster, environmentally friendly and cost-effective for the quantification of ketamine and norketamine in urine samples. To our knowledge, this is the first work that employs a high throughput based microextraction approach for the simultaneous extraction and subsequent desorption of ketamine and norketamine in up to 100 urine samples simultaneously.

scholarly journals A Novel Bioanalytical Method for the Determination of Opioids in Blood and Pericardial Fluid

2020 ◽  
Vol 44 (8) ◽  
pp. 754-768
Author(s):  
Elisa Ferreira ◽  
Francisco Corte Real ◽  
Teresa Pinho e Melo ◽  
Cláudia Margalho
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Hydroxylamine Hydrochloride ◽  
Pericardial Fluid ◽  
Gas Chromatography Mass Spectrometry ◽  
Forensic Sciences ◽  
Selected Ion Monitoring ◽  
Intermediate Precision ◽  
Analytical Methodology

Abstract Opioids are the drugs most commonly detected in overdose deaths and the second most consumed worldwide. An analytical methodology has been optimized and fully validated for the determination of codeine, morphine, 6-acetylmorphine, 6-acetylcodeine, oxycodone, oxymorphone and fentanyl in whole blood and pericardial fluid. The internal standards used were codeine-d3, morphine-d3, 6-acetylmorphine-d3 and fentanyl-d5. Before solid-phase extraction, volumes of 250 μL of blood and pericardial fluid were subjected to a protein precipitation (with 750 μL of ice-cold acetonitrile) and a microwave-induced oximation was performed using a solution of 1% aqueous hydroxylamine hydrochloride in phosphate-buffered saline (1:2, v/v). Finally, the dried extracts were further derivatized with a solution of n-methyl-n-(trimethylsilyl) trifluoroacetamide + 5% trimethylchlorosilane under microwave irradiation. The chromatographic analysis was carried out using gas chromatography–mass spectrometry operating in electron impact and selected ion monitoring mode. For all analytes, the method was linear between 5 and 1,000 ng/mL with determination coefficients (r2) >0.99. Depending on the analyte and matrix, the limit of detection varies between 3 and 4 ng/mL. Intra- and intermediate precision (<20%) and bias (±20%) were acceptable for all analytes in both matrices. The stability of the substances in the studied matrices was guaranteed, at least, 24 h in the autosampler, 4 h at room temperature and 30 days after three freeze/thaw cycles. This methodology was applied to real samples from the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

Determination of Halogenated Contaminants in Human Adipose Tissue

1986 ◽  
Vol 69 (3) ◽  
pp. 451-458
Author(s):  
Guy L Lebel ◽  
David T Williams
Keyword(s):  
Gas Chromatography ◽  
Adipose Tissue ◽  
Methylene Chloride ◽  
Gel Permeation Chromatography ◽  
Human Adipose Tissue ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Fat Extraction ◽  
Capillary Column Gas Chromatography

Abstract <A method has been developed for determination of organochlorine contaminants in human adipose tissue. After fat extraction from the tissue with acetone-hexane (15 + 85, v/v), organochlorines were fractionated from fat by gel permeation chromatography with methylene chloride-cyclohexane (1 + 1, v/v) as solvent. After Florisil column cleanup, the GPC extract was analyzed by capillary column gas chromatography using 2 columns of different polarity. Compound identity was confirmed by gas chromatography-mass spectrometry using selected ion monitoring. Recoveries for fortification levels of 10-500 ng/g were greater than 80 % except for trichlorobenzene and hexachlorobutadiene (ca 60%).

Gas Chromatographic-Mass Spectrometric Determination of Six Sulfonamide Residues in Egg and Animal Tissues

1990 ◽  
Vol 73 (6) ◽  
pp. 886-892 ◽  
Author(s):  
Keigo Takatsuki ◽  
Tadashi Kikuchi
Keyword(s):  
Methylene Chloride ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometric Method ◽  
Mass Spectrometric Method ◽  
Animal Tissues ◽  
Selected Ion Monitoring ◽  
Ether Solution ◽  
Sulfonamide Residues

Abstract A gas chromatographlc-mass spectrometric method using selected Ion monitoring mode for simultaneous determination of 6 sulfonamides in egg and edible animal tissues has been developed. Sulfonamides are extracted from a sample with acetonltrlle. The extract Is passed through a silica cartridge column and concentrated. Dlazomethane in ether Is added to methylate sulfonamides. After evaporation, the residue Is dissolved In methylene chloride and cleaned up by silica gel column chromatography. The methylene chloride eluate containing sulfonamide-methyl derivatives Is evaporated to dryness, redlssolved In ether and partitioned between 6N hydrochloric acid. The acid phase is made alkaline, extracted with ether, and the ether solution, after concentration, Is analyzed by gas chromatography-mass spectrometry in selected Ion monitoring mode. Average recoveries from egg and silver salmon fortified at 1 and 0.2 ppm levels with 6 sulfonamides are 99.2 and 84.3%, respectively; coefficients of variation are 7.03 and 11.20%, respectively. Detection limits are 0.01-0.05 ppm.

scholarly journals Determination of Mammalian Lignans in Biological Samples by Modified Gas Chromatography/Mass Spectrometry

2007 ◽  
Vol 90 (3) ◽  
pp. 641-646 ◽  
Author(s):  
Ajay Bommareddy ◽  
Bhanu L Arasada ◽  
Duane P Mathees ◽  
Chandradhar Dwivedi
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Serum Samples ◽  
Selected Ion Monitoring ◽  
Beneficial Effects ◽  
Chromatography Mass Spectrometry ◽  
Flaxseed Meal

Abstract Lignans in flaxseed have been part of the human diet for centuries. In 1955, the isolation and structure of the lignan derivative secoisolariciresinol diglucoside (SDG) was reported. The biological role of SDG and mammalian lignan metabolites enterodiol and enterolactone was initially reported 20 years later. Experimental evidences showed the beneficial effects of lignans on breast, colon, and thyroid cancer. A modified gas chromatography/mass spectrometry (GC/MS) assay was developed for lignans in serum and colon samples of rats fed flaxseed meal. The method developed for the analysis of metabolites involves extraction and derivatization of samples and quantitative analysis by selected ion monitoring using GC/MS. The levels of lignan metabolites enterodiol and enterolactone were determined to be 0.013 and 0.23 M in serum samples and 0.008 and 1.63 M in colon samples.

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