Simultaneous determination of drugs and pesticides in postmortem blood using dispersive solid-phase extraction and large volume injection-programmed temperature vaporization-gas chromatography–mass spectrometry

Júnior, Ettore Ferrari; Caldas, Eloísa Dutra

doi:10.1016/j.forsciint.2018.07.031

Cited by 36 publications

(10 citation statements)

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“…The initial step of this work was establishing the instrumental conditions that better fit the compounds under study. A mix solution of six TCAs was analyzed by GC-MS operating in the full-scan mode acquisition, which allowed to obtain the target ions (base peaks) and quantifier ions, also in accordance with the literature ( Table 1 ) [ 24 , 25 , 26 , 27 ]. The obtained chromatogram by LVI-GC-MS(SIM) showed symmetrical peak shapes in less than 20 min of running time.…”

Section: Resultsmentioning

confidence: 99%

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

et al. 2021

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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.

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Section: Resultsmentioning

confidence: 99%

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

et al. 2021

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“…Four extraction protocols were tested based on previous work conducted by our research group [7], varying the amount of water and ACN (− 20 °C): protocol 1 (P1) (1 mL of ACN and 1 mL of water); protocol 2 (P2) (0.5 mL of ACN and 1 mL of water); protocol 3 (P3) (1 mL of ACN and 0.5 mL of water); and protocol 4 (P4) (0.5 mL of ACN and 0.5 mL of water). In all cases, 500 µL of biological fluid (urine or blood) and 20 µL of the IS mix were added to a 15 mL falcon-type tube (two glass beads were also added to the tubes containing blood).…”

Section: Sample Extraction and Clean-upmentioning

confidence: 99%

“…In Brazil, data on NPS are scarce, but include seizure data [4,5] and some postmortem cases [6]. Furthermore, prescription drugs are among the major causes of fatal poisonings in the world, and their concomitant use with illegal drugs is common [7][8][9].…”

Section: Introductionmentioning

confidence: 99%

“…Blood is the most used biological material to evaluate the role of a drug in modifying human performance and behavior [10] and to investigate intoxication cases [7,11]. Urine has a larger detection window when compared to other biological specimens, and is the main matrix used in different areas of analytical toxicology, such as doping, workplace drug testing, and screening analysis in clinical and forensic toxicology [12].…”

Section: Introductionmentioning

confidence: 99%

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Determination of new psychoactive substances and other drugs in postmortem blood and urine by UHPLC–MS/MS: method validation and analysis of forensic samples

Júnior

Caldas

2021

Forensic Toxicol

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Purpose This study aimed to validate a modified QuEChERS method followed by ultra-high performance liquid chromatography-tandem mass spectrometry to determine 79 new psychoactive substances (NPS) and other drugs in blood and urine. Methods Prescription drugs (n = 23), synthetic cathinones (n = 13), phenethylamines (n = 11); synthetic cannabinoids (n = 8), amphetamines (n = 7) and other psychoactive substances (n = 17) were included in the method. 500 µL of biological fluid was extracted with 2 mL of water/ACN (1:1), 500 mg of anhydrous MgSO 4 /NaOAc (4:1) added, followed by a supernatant cleanup with 25 mg of primary secondary amine and 75 mg of anhydrous MgSO 4 . Quantification was done using matrixmatched calibration curves and deuterated internal standards. ResultsThe method was satisfactorily validated for blood and urine at limit of quantifications ranging from 0.4 to 16 ng/ mL, and applied to the analysis of 54 blood (38 postmortem and 16 antemortem) and 16 antemortem urine samples from 68 forensic cases. All urine samples and 59.3% of the blood samples were positive for at least one analyte. Twenty-two analytes were detected in at least one biological sample, including the synthetic cathinones ethylone (222 ng/mL, antemortem blood), eutylone (246 and 446 ng/mL, urine), and N-ethylpentylone (597 and 7.3 ng/mL, postmortem and antemortem blood, respectively). Conclusions The validated method was shown to be suitable for the analysis of blood and urine forensic samples and an important tool to collect information on emerging drug threats and understanding the impact of NPS and other drugs in poisoning cases.

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“…A d-SPE protocol based on the modified QuEChERS procedure (using 50 mg of PSA and 150 mg of anhydrous MgSO 4 ), followed by large volume injection programmed temperature vaporization (LVI-PTV)-gas chromatography-mass spectrometry (GC-MS) analysis, was developed for the simultaneous determination of 16 drugs and pesticides in postmortem blood samples without derivatization [46]. The validated d-SPE/LVI-PTV/GC-MS method is suitable for routine analysis in a forensic laboratory.…”

Section: Solid-phase Extractionsmentioning

confidence: 99%

Modern Approaches to Preparation of Body Fluids for Determination of Bioactive Compounds

Madej

Piekoszewski

2019

Separations

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The current clinical and forensic toxicological analysis of body fluids requires a modern approach to sample preparation characterized by high selectivity and enrichment capability, suitability for micro-samples, simplicity and speed, and the possibility of automation and miniaturization, as well as the use of small amounts of reagents, especially toxic solvents. Most of the abovementioned features may be realized using so-called microextraction techniques which cover liquid-phase techniques (e.g., single-drop microextraction, SDME; dispersive liquid–liquid microextraction, DLLME; hollow-fiber liquid-phase microextraction, HF-LPME) and solid-phase extraction techniques (solid-phase microextraction, SPME; microextraction in packed syringes, MEPS; disposable pipette tip extraction, DPX; stir bar sorption extraction, SBSE). Some other extraction methodologies like dispersive solid-phase extraction (d-SPE) or magnetic solid-phase extraction (MSPE) can also be easily miniaturized. This review briefly describes and characterizes the abovementioned extraction methods, and then presents their current applications to the preparation of body fluids analyzed for bioactive compounds in combination with appropriate analytical methods, mainly chromatographic and related techniques. The perspectives of the analytical area we are interested in are also indicated.

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Simultaneous determination of drugs and pesticides in postmortem blood using dispersive solid-phase extraction and large volume injection-programmed temperature vaporization-gas chromatography–mass spectrometry

Cited by 36 publications

References 45 publications

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

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

Determination of new psychoactive substances and other drugs in postmortem blood and urine by UHPLC–MS/MS: method validation and analysis of forensic samples

Modern Approaches to Preparation of Body Fluids for Determination of Bioactive Compounds

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