Your browser doesn't support javascript.
loading
Show: 20 | 50 | 100
Results 1 - 20 de 91
Filter
1.
Mikrochim Acta ; 189(2): 52, 2022 01 08.
Article in English | MEDLINE | ID: mdl-35000010

ABSTRACT

A poly(methacrylic acid-co-ethylene glycol dimethacrylate)-based magnetic sorbent was used for the rapid and sensitive determination of tricyclic antidepressants and their main active metabolites in human urine. This material was characterized by magnetism measurements, zeta potential, scanning electron microscopy, nitrogen adsorption-desorption isotherms, and thermogravimetric analysis. The proposed analytical method is based on stir bar sorptive-dispersive microextraction (SBSDME) followed by liquid chromatography-tandem mass spectrometry. The main parameters involved in the extraction step were optimized by using the response surface methodology as a multivariate optimization method, whereas a univariate approach was employed to study the desorption parameters. Under the optimized conditions, the proposed method was properly validated showing good linearity (at least up to 50 ng mL-1) and enrichment factors (13-22), limits of detection and quantification in the low ng L-1 range (1.4-7.0 ng L-1), and good intra- and inter-day repeatability (relative standard deviations below 15%). Matrix effects were observed for the direct analysis of urine samples, but they were negligible when a 1:1 v/v dilution with deionized water was performed. Finally, the method was successfully applied to human urine samples from three volunteers, one of them consuming a prescribed drug for depression that tested positive for clomipramine and its main active metabolite. Quantitative relative recoveries (80-113%) were obtained by external calibration. The present work expands the applicability of the SBSDME to new analytes and new types of magnetic sorbents.


Subject(s)
Antidepressive Agents, Tricyclic , Polymethacrylic Acids , Solid Phase Microextraction , Humans , Antidepressive Agents, Tricyclic/chemistry , Antidepressive Agents, Tricyclic/metabolism , Antidepressive Agents, Tricyclic/urine , Chromatography, Liquid , Cobalt/chemistry , Ferric Compounds/chemistry , Magnetic Phenomena , Polymethacrylic Acids/chemistry , Silicon Dioxide/chemistry , Solid Phase Microextraction/methods , Tandem Mass Spectrometry
2.
Mikrochim Acta ; 188(3): 73, 2021 02 06.
Article in English | MEDLINE | ID: mdl-33550423

ABSTRACT

Gelatin microsphere-coated Fe3O4@graphene quantum dots (Fe3O4@GQD@GM) were designed and synthesized as a novel sorbent via ultrasonic-assisted dispersive magnetic solid-phase extraction (UA-DMSPE) method. The synthesized sorbent was identified and confirmed by FT-IR, XRD, VSM, and SEM techniques. UA-DMSPE was combined with corona discharge ion mobility spectrometry for trace determination of desipramine, sertraline, and citalopram. Effective parameters were considered and optimized. The proposed method, under optimal conditions, showed excellent linearity in different concentration ranges (2-700 ng mL-1, R2 > 0.995), repeatability (RSD < 5.1%), good sensitivity (LODs in the range 0.6-1.5 ng mL-1), high preconcentration factor (PF = 207-218), and acceptable relative recoveries (93.5-101.8%). Eventually, this method was used to determine tricyclic antidepressants in various biological samples. Schematic presentation of the microextraction and monitoring of TCAs by ultrasonic-assisted dispersive magnetic solid phase microextraction-ion mobility spectrometry producer.


Subject(s)
Antidepressive Agents, Tricyclic/isolation & purification , Microspheres , Nanocomposites/chemistry , Quantum Dots/chemistry , Solid Phase Extraction/methods , Adsorption , Antidepressive Agents, Tricyclic/blood , Antidepressive Agents, Tricyclic/chemistry , Antidepressive Agents, Tricyclic/urine , Citalopram/blood , Citalopram/chemistry , Citalopram/isolation & purification , Citalopram/urine , Desipramine/blood , Desipramine/chemistry , Desipramine/isolation & purification , Desipramine/urine , Gelatin/chemistry , Graphite/chemistry , Humans , Limit of Detection , Magnetic Phenomena , Magnetite Nanoparticles/chemistry , Sertraline/blood , Sertraline/chemistry , Sertraline/isolation & purification , Sertraline/urine
3.
Molecules ; 26(11)2021 May 22.
Article in English | MEDLINE | ID: mdl-34067333

ABSTRACT

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.


Subject(s)
Antidepressive Agents, Tricyclic/urine , Solid Phase Microextraction/methods , Urinalysis/methods , Adsorption , Biocompatible Materials/chemistry , Charcoal/chemistry , Gas Chromatography-Mass Spectrometry , Humans , Hydrogen-Ion Concentration , Ions , Limit of Detection , Liquid Phase Microextraction/methods , Polymers/chemistry , Polypropylenes/chemistry , Reproducibility of Results , Urinalysis/standards , Water/chemistry
4.
Biomed Chromatogr ; 33(11): e4642, 2019 Nov.
Article in English | MEDLINE | ID: mdl-31273813

ABSTRACT

Sodium sulfate-induced deep eutectic solvent-based solidification of floating organic droplets-dispersive liquid phase microextraction was developed prior to gas chromatography-mass spectrometry. In this method, a mixture of Na2 SO4 solution (as phase separation agent and disperser) containing menthol-decanoic acid was rapidly injected into an alkaline aqueous solution containing Na2 SO4 . The solution was placed in an ice bath and the menthol-decanoic acid solvent was solidified on the surface of the solution. Under the optimal conditions, the enrichment factors and extraction recoveries were 122-147 and 74-89%, respectively. Finally, an aliquot of the collected organic phase was removed and mixed with acetonitrile and injected into the separation system. The limits of detection and lower limits of quantification were obtained at the ranges of 13-25 and 24-41 ng L-1 , respectively. The relative standard deviations of the proposed method were ≤11% for intra- and inter-day precisions at four concentrations.


Subject(s)
Antidepressive Agents, Tricyclic/isolation & purification , Liquid Phase Microextraction/methods , Sulfates/chemistry , Antidepressive Agents, Tricyclic/urine , Gas Chromatography-Mass Spectrometry , Green Chemistry Technology , Humans , Limit of Detection , Linear Models , Reproducibility of Results
5.
Electrophoresis ; 37(2): 339-46, 2016 Jan.
Article in English | MEDLINE | ID: mdl-26462723

ABSTRACT

Electromembrane extraction (EME) of model analytes was carried out using a virtually rotating supported liquid membrane (SLM). The virtual (nonmechanical) rotating of the SLM was achieved using a novel electrode assembly including a central electrode immersed inside the lumen of the SLM and five counter electrodes surrounding the SLM. A particular electronic circuit was designed to distribute the potential among five counter electrodes in a rotating pattern. The effect of the experimental parameters on the recovery of the extraction was investigated for verapamil (VPL), trimipramine (TRP), and clomipramine (CLP) as the model analytes and 2-ethyl hexanol as the SLM solvent. The results showed that the recovery of the extraction is a function of the angular velocity of the virtual rotation. The best results were obtained at an angular velocity of 1.83 RadS(-1) (or a rotation frequency of 0.29 Hz).The optimization of the parameters gave higher recoveries up to 50% greater than those of a conventional EME method. The rotating also allowed the extraction to be carried out at shorter time (15 min) and lower voltage (200 V) with respect to the conventional extraction. The model analytes were successfully extracted from wastewater and human urine samples with recoveries ranging from 38 to 85%. The RSD of the determinations was in the range of 12.6 to 14.8%.


Subject(s)
Chemical Fractionation/instrumentation , Clomipramine/isolation & purification , Electrochemical Techniques/instrumentation , Membranes, Artificial , Trimipramine/isolation & purification , Verapamil/isolation & purification , Anti-Arrhythmia Agents/isolation & purification , Anti-Arrhythmia Agents/urine , Antidepressive Agents, Tricyclic/isolation & purification , Antidepressive Agents, Tricyclic/urine , Clomipramine/urine , Electrodes , Equipment Design , Humans , Limit of Detection , Rotation , Trimipramine/urine , Urinalysis/instrumentation , Verapamil/urine , Wastewater/analysis , Water Pollutants, Chemical/isolation & purification , Water Pollutants, Chemical/urine , Water Purification/instrumentation
6.
Anal Bioanal Chem ; 408(27): 7719-7729, 2016 Nov.
Article in English | MEDLINE | ID: mdl-27562753

ABSTRACT

Ultrasonic-assisted magnetic dispersive solid-phase microextraction coupled with high performance liquid chromatography has been developed for extraction and determination of mirtazapine, N-desmethyl mirtazapine, and 8-hydroxy mirtazapine in human urine and water samples. Magnetic graphene oxide-polyaniline nanocomposite (MGOPA) as a novel SPME sorbent was synthesized and used for the microextraction process. The analytical performance of MGOPA was compared with magnetic graphene oxide nanocomposite and indicated that the new sorbent was quite effective for extraction of mirtazapine, N-desmethyl mirtazapine, and 8-hydroxy mirtazapine. A two-stage experimental design approach, Plackett-Burman screening design and Box-Behnken optimization design, was used for screening and optimizing of significant variables in the microextraction process. The practical applicability of the proposed method was assessed by studying the linearity, intra-day and inter-day accuracy, enrichment factor, and precision. This method can be satisfactorily applied to the determination of mirtazapine and its metabolites in human urine and environmental water samples. Graphical Abstract Magnetic graphene oxide-polyaniline nanocomposite.


Subject(s)
Antidepressive Agents, Tricyclic/urine , Mianserin/analogs & derivatives , Solid Phase Microextraction/methods , Water Pollutants, Chemical/analysis , Adsorption , Aniline Compounds/chemistry , Chromatography, High Pressure Liquid , Factor Analysis, Statistical , Fresh Water/chemistry , Graphite/chemistry , Healthy Volunteers , Humans , Magnets , Mianserin/urine , Mirtazapine , Nanocomposites/chemistry , Oxides/chemistry , Sonication
7.
Mo Med ; 112(3): 206-10, 2015.
Article in English | MEDLINE | ID: mdl-26168592

ABSTRACT

Urine drug screens are commonly used in various clinical settings and situations. Immunoassays are the most commonly available method of testing for urine drug screens in hospitals. Although convenient, immunoassays are prone to false positive and false negative results. It is important for the health care provider to understand the principles of the laboratory methods involved with urine drug screens as this will help guide appropriate result interpretation and therefore improve clinical care.


Subject(s)
Narcotics/urine , Substance Abuse Detection/methods , Antidepressive Agents, Tricyclic/urine , Emergency Medicine , Humans
8.
Sud Med Ekspert ; 58(1): 31-34, 2015.
Article in Russian | MEDLINE | ID: mdl-25874316

ABSTRACT

Tricyclic antidepressants are among the preparations that most frequently cause intoxication in adults and children; moreover, poisoning with these substances not infrequently has a fatal outcome. Medications belonging to this group, such as amitriptyline, are extensively used to manage manifestations of depression, anxiety, migraine, neuropathic pain, and hyperactivity syndrome. Amitriptyline overdosage causes non-specific symptoms of intoxication, and its clinical picture does not allow to identify the nature of a psychotropic xenobiotic. Of primary importance in connection with this is to establish the cause of intoxication or death by the clinical toxicological and forensic medical methods based on the results of the fast identification and quantitation of amitriptyline in biological materials including blood, urine, hepatic tissues, etc. The authors describe the method for the determination of amitriptyline and its principal physiological metabolite nortriptyline in biological objects with the help of high performance liquid chromatography (HPLC).


Subject(s)
Amitriptyline/analysis , Antidepressive Agents, Tricyclic/analysis , Forensic Toxicology/methods , Liver/metabolism , Nortriptyline/analysis , Amitriptyline/blood , Amitriptyline/poisoning , Amitriptyline/urine , Antidepressive Agents, Tricyclic/blood , Antidepressive Agents, Tricyclic/poisoning , Antidepressive Agents, Tricyclic/urine , Cadaver , Calibration , Chromatography, High Pressure Liquid , Humans , Limit of Detection , Liver/pathology , Nortriptyline/blood , Nortriptyline/urine , Postmortem Changes
9.
Pain Med ; 15(3): 355-63, 2014 Mar.
Article in English | MEDLINE | ID: mdl-24308804

ABSTRACT

OBJECTIVE: Tricyclic antidepressants (TCAs) are first-line treatment for neuropathic pain. Despite widespread use, many health care providers do not know which patients are currently taking TCAs. The objective of this retrospective data analysis was to determine adherence rates to amitriptyline, nortriptyline, or imipramine. The rate at which patients used TCAs (confirmed by presence of TCA in the urine) but did not inform their health care provider is also reported (non-informed prescriber rate). Finally, the effects of age, sex, and number of prescriptions on adherence and non-informed prescriber rates were assessed. METHODS: Urinary excretion data were obtained from 55,296 patients with pain and were analyzed using liquid chromatography tandem mass spectrometry in a multiplex assay which included amitriptyline, nortriptyline, and imipramine. RESULTS: The adherence rate was 66% (1,407/2,137); the rate of non-informed prescribers was 3% (1,547/55,296) among the general population, and 52% (1,547/2,954) when only TCA users were considered. While adherence was higher among older and female subjects, the number of other medications did not affect adherence rate. CONCLUSIONS: This analysis reveals that many prescribers are not informed when patients start and stop using TCAs.


Subject(s)
Amitriptyline/urine , Antidepressive Agents, Tricyclic/therapeutic use , Imipramine/urine , Nortriptyline/urine , Pain/drug therapy , Adolescent , Adult , Age Factors , Aged , Antidepressive Agents, Tricyclic/urine , Drug Interactions , Female , Humans , Male , Middle Aged , Retrospective Studies , Sex Factors , Young Adult
10.
Sud Med Ekspert ; 57(1): 37-40, 2014.
Article in Russian | MEDLINE | ID: mdl-25275184

ABSTRACT

The present study was designed to estimate the effectiveness of isolation of mirtazapine from the liver, blood, and urine. The conditions were developed for the identification and quantitative measurement of the isolated mirtazapine with the use of high performance liquid chromatography and detection from the UV-spectrum and mass-spectrometry. The retention time of mirtazapine isolated from the liver was 2.88 +/- 0.08 min. The straight-line equation within the range of mirtazapine concentrations from 1 to 20 mc/ml was characterized by the dependence: Y = 3.25 x 10(4)X - 6.27 x 10(3) (r = 0.9997). The study showed that it is possible to isolate 46.44 +/- 1.89% of mirtazapine present in the liver and 50.4 +/- 1.05% from blood using extraction by acetonitrile acidified with an 1 M hydrochloric acid solution. Chloroform extraction from urine at pH 7.0-8.0 releases 90.22 +/- 1.88% of mirtazapine.


Subject(s)
Antidepressive Agents, Tricyclic/analysis , Forensic Toxicology/methods , Liver/chemistry , Mianserin/analogs & derivatives , Antidepressive Agents, Tricyclic/blood , Antidepressive Agents, Tricyclic/urine , Cadaver , Chromatography, High Pressure Liquid , Female , Humans , Liver/metabolism , Liver/pathology , Male , Mass Spectrometry , Mianserin/analysis , Mianserin/blood , Mianserin/urine , Mirtazapine , Sensitivity and Specificity
11.
Analyst ; 138(5): 1395-404, 2013 Mar 07.
Article in English | MEDLINE | ID: mdl-23324861

ABSTRACT

An Amberlite XAD-2 (XAD2) and titanium dioxide nanoparticles (TNPs) modified glassy carbon paste electrode (XAD2-TNP-GCPE) was developed for the determination of imipramine (IMI), trimipramine (TRI) and desipramine (DES). The electrochemical behavior of these molecules was investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping differential pulse voltammetry (AdSDPV). After optimization of analytical conditions using a XAD2-TNP-GCPE electrode at pH 6.0 phosphate buffer (0.1 M), the peak currents were found to vary linearly with its concentration in the range of 1.30 × 10(-9) to 6.23 × 10(-6) M for IMI, 1.16 × 10(-9) to 6.87 × 10(-6) M for TRI and 1.43 × 10(-9) to 5.68 × 10(-6) M for DES. The detection limits (S/N = 3) of 3.93 × 10(-10), 3.51 × 10(-10) and 4.35 × 10(-10) M were obtained for IMI, TRI and DES respectively using AdSDPV. The prepared modified electrode showed several advantages such as a simple preparation method, high sensitivity, very low detection limits and excellent reproducibility. The proposed method was employed for the determination of IMI, TRI and DES in pharmaceutical formulations, blood serum and urine samples.


Subject(s)
Antidepressive Agents, Tricyclic/analysis , Desipramine/analysis , Electrochemical Techniques/methods , Imipramine/analysis , Trimipramine/analysis , Adsorption , Antidepressive Agents, Tricyclic/blood , Antidepressive Agents, Tricyclic/urine , Carbon/chemistry , Desipramine/blood , Desipramine/urine , Electrodes , Humans , Imipramine/blood , Imipramine/urine , Limit of Detection , Nanoparticles/chemistry , Pharmaceutical Preparations/chemistry , Reproducibility of Results , Resins, Synthetic/chemistry , Titanium/chemistry , Trimipramine/blood , Trimipramine/urine
12.
J Sep Sci ; 36(14): 2315-22, 2013 Jul.
Article in English | MEDLINE | ID: mdl-23661273

ABSTRACT

In this study, a platinum wire coated with poly(3,4-ethylenedioxythiophen) was used as an electro-assisted solid-phase microextraction fiber for the quantification of tricyclic antidepressant drugs in biological samples by coupling to GC employing a flame ionization detector. In this study, an electric field increased the extraction rate and recovery. The fiber used as a solid phase was synthesized by the electropolymerization of 3,4-ethylenedioxythiophen monomers onto a platinum wire. The ability of this fiber to extract imipramine, desipramine, and clomipramine by using the electro-assisted solid-phase microextraction technique was evaluated. The effect of various parameters that influence the extraction efficiency, which include solution temperature, extraction time, stirring rate, ionic strength, time and temperature of desorption, and thickness of the fiber, was optimized. Under optimized conditions, the linear ranges and regression coefficients of calibration curves were in the range of 0.5-250 and 0.990-0.998 ng/mL, respectively. Detection limits were in the range of 0.15-0.45 ng/mL. Finally, this method was applied to the determination of drugs in urine and wastewater samples and recoveries were 4.8-108.9%.


Subject(s)
Antidepressive Agents, Tricyclic/isolation & purification , Antidepressive Agents, Tricyclic/urine , Chromatography, Gas/methods , Solid Phase Microextraction/methods , Bridged Bicyclo Compounds, Heterocyclic/chemistry , Humans , Hydrogen-Ion Concentration , Limit of Detection , Polymers/chemistry , Solid Phase Microextraction/instrumentation
13.
J Clin Lab Anal ; 26(4): 286-94, 2012 Jul.
Article in English | MEDLINE | ID: mdl-22811363

ABSTRACT

A sensitive, specific, and rapid high-pressure liquid chromatography/mass spectrometry/mass spectrometry method was developed for the quantitation of 11 tricyclic antidepressants and/or their metabolites; fluoxetine and norfluoxetine; cyclobenzaprine; and trazodone in urine. Samples were alkalinized with 0.2 N NaOH and extracted into 2 ml of hexane: ethyl acetate (1:1), evaporated to dryness, and reconstituted with 100 µl of 20 mM ammonium formate: methanol (20:80). The chromatographic separation was performed using an Allure Biphenyl 100 × 3.2 mm, 5-µ column with a mobile phase consisting of 20 mM ammonium formate: methanol (20:80 v/v) at a flow rate of 0.5 ml/min. The detection was accomplished by multiple-reaction monitoring via electrospray ionization source operating in the positive ionization mode. The calibration curve was linear over the investigated concentration range, 25-2,000 ng/ml, for each analyte using 1.0 ml of urine. The lower limit of quantitation for each analyte was 25 ng/ml. The intra- and inter-day precisions had coefficient of variation less than 15% and the accuracy was within the range from 88% to 109%. The method proved adequate for the tricyclic antidepressants analysis of urine for emergency clinical toxicology and pain management compliance testing.


Subject(s)
Antidepressive Agents, Tricyclic/urine , Chromatography, High Pressure Liquid/methods , Pain Management/methods , Pain/drug therapy , Pain/urine , Patient Compliance , Tandem Mass Spectrometry/methods , Antidepressive Agents, Tricyclic/chemistry , Humans , Reproducibility of Results , Sensitivity and Specificity
14.
Pediatr Emerg Care ; 28(10): 1066-9, 2012 Oct.
Article in English | MEDLINE | ID: mdl-23034495

ABSTRACT

BACKGROUND: Tricyclic antidepressant (TCA) ingestions are a relatively common pediatric ingestion, with significant potential for both cardiac and neurological toxicity. Previous studies on pediatric TCA ingestions have found the threshold of toxicity to be 5 mg/kg. CASE: We report a case of an 8-year-old girl who presented to the emergency department with depressed mental status and seizure-like movements. An extensive workup was pursued to evaluate the cause of her mental status, which only revealed a positive urine toxicology screen for TCA. Quantified serum levels of amitriptyline were 121 ng/mL (therapeutic range, 50-300 ng/mL) and nortriptyline were 79 ng/mL (therapeutic range 70-170 ng/mL), 18 hours after onset of symptoms. Subsequent history obtained after her mental status returned to normal revealed that she had ingested amitriptyline at a dose of 0.8 mg/kg. CONCLUSIONS: Tricyclic antidepressant ingestion has a high potential for toxicity in pediatric patients. This case suggests, contrary to previous literature, that toxicity may occur even with small doses.


Subject(s)
Amitriptyline/poisoning , Antidepressive Agents, Tricyclic/poisoning , Depression/chemically induced , Triage/methods , Administration, Oral , Amitriptyline/administration & dosage , Amitriptyline/urine , Antidepressive Agents, Tricyclic/administration & dosage , Antidepressive Agents, Tricyclic/urine , Child , Depression/diagnosis , Depression/urine , Diagnosis, Differential , Dose-Response Relationship, Drug , Female , Humans , Urinalysis
15.
Leg Med (Tokyo) ; 48: 101804, 2021 Feb.
Article in English | MEDLINE | ID: mdl-33152676

ABSTRACT

The efficacy of DRIVEN-FLOW® M7-II(DFM7II) for seven drug groups was compared with Triage DOA® (Triage) using 340 autopsy urine samples taken from bodies within 1 month of death based on mass screening analysis of GC/MS and LC-MS/MS. The sensitivity to benzodiazepines was 0.56 in Triage and 0.53 in DFM7II with few false positives, and their accuracy was 0.88. Triage detected triazolo diazepine derivatives more easily than DFM7II. DFM7II detected diazepam and nitro benzodiazepines more easily than Triage. There were nine amphetamine false-positive cases of more than 10 days after death in Triage, but these were absent in DFM7II during this period. The accuracy of amphetamines for Triage was 0.96 and for DFM7II was 1. Tricyclic antidepressant (TCA) was detected in five cases by mass analysis, while there were four false-positive cases using Triage and eight cases using DFM7II. In the TCA false-positive cases of both kits, tricyclic psychotics such as chlorpromazine, carbamazepine, and quetiapine were included as well as the drug poisoning cases. There were no samples containing cocaine or THC. The accuracy of DFM7II for opiate and barbiturates was 1, but those of Triage was less than 1. Based on the above, DFM7II is a more accurate kit with fewer false-positives for target drug groups, other than TCA, than Triage.


Subject(s)
Amphetamine/urine , Antidepressive Agents, Tricyclic/urine , Autopsy/methods , Azepines/urine , Benzodiazepines/urine , Forensic Medicine/methods , Reagent Kits, Diagnostic , Substance Abuse Detection/methods , Triazoles/urine , False Positive Reactions , Humans , Sensitivity and Specificity
16.
J Sep Sci ; 33(2): 268-76, 2010 Feb.
Article in English | MEDLINE | ID: mdl-20087868

ABSTRACT

A selective and reproducible off-line solid-phase microextraction procedure was developed for the simultaneous enantioselective determination of mirtazapine (MRT), demethylmirtazapine and 8-hydroxymirtazapine in human urine. CE was used for optimization of the extraction procedure whereas LC-MS was used for method validation and application. The influence of important factors in the solid-phase microextraction efficiency is discussed, such as the fiber coatings, extraction time, pH, ionic strength, temperature and desorption time. Before extraction, human urine samples were submitted to enzymatic hydrolysis at 37 degrees C for 16 h. Then, the enzyme was precipitated with trichloroacetic acid and the pH was adjusted to 8 with 1 mol/L pH 11 phosphate buffer solution. In the extraction, the analytes were transferred from the aqueous solution to the polydimethylsiloxane-divinylbenzene fiber coating and then desorbed in methanol. The mean recoveries were 5.4, 1.7 and 1.0% for MRT, demethylmirtazapine and 8-hydroxymirtazapine enantiomers, respectively. The method was linear over the concentration range of 62-1250 ng/mL. The within-day and between-day assay precision and accuracy were lower than 15%. The method was successfully employed in a preliminary cumulative urinary excretion study after administration of racemic MRT to a healthy volunteer.


Subject(s)
Mianserin/analogs & derivatives , Solid Phase Microextraction/methods , Antidepressive Agents, Tricyclic/administration & dosage , Antidepressive Agents, Tricyclic/analysis , Antidepressive Agents, Tricyclic/pharmacokinetics , Antidepressive Agents, Tricyclic/urine , Buffers , Chromatography, Liquid , Humans , Hydrogen-Ion Concentration , Mianserin/administration & dosage , Mianserin/isolation & purification , Mianserin/pharmacokinetics , Mianserin/urine , Mirtazapine , Osmolar Concentration , Reproducibility of Results , Solid Phase Microextraction/instrumentation , Stereoisomerism , Tandem Mass Spectrometry
17.
Anal Chim Acta ; 1105: 95-104, 2020 Apr 08.
Article in English | MEDLINE | ID: mdl-32138931

ABSTRACT

In this study, an electromembrane extraction-dispersive liquid-liquid microextraction (EME-DLLME) was performed using a lab-on-a-disc device. It was used for sample microextraction, preconcentration, and quantitative determination of tricyclic antidepressants as model analytes in biofluids. The disc consisted of six extraction units for six parallel extractions. First, 100 µL of a biofluid was used to extract the analytes by the drop-to-drop EME to clean-up the sample. The extraction then was followed by applying the DLLME method to preconcentrate the analytes and make them ready for being analyzed by gas chromatography (GC). Implementing the EME-DLLME method on a chip device brought some significant advantages over the conventional methods, including saving space, cost, and materials as well as low sample and energy consumption. In the designed device, centrifugal force was used to move the fluids in the disc. Both sample preparation methods were performed on the same disc without manual transference of the donor phases for doing the two methods. Scalable centrifugal force made it possible to adjust the injection speed of the organic solvent into the aqueous solution in the DLLME step by changing the spin speed. Spin speed of 100 rpm was used in dispersion step and spin speed of 3500 rpm was used to sediment organic phase in DLLME step. The proposed device provides effective and reproducible extraction using a low volume of the sample solution. After optimization of the effective parameters, an EME-DLLME followed by GC-MS was performed for determination of amitriptyline and imipramine in saliva, urine, and blood plasma samples. The method provides extraction recoveries and preconcentration factors in the range of 43%-70.8% and 21.5-35.5 respectively. The detection limits less than 0.5 µg L-1 with the relative standard deviations of the analysis which were found in the range of 1.9%-3.5% (n = 5). The method is suitable for drug monitoring and analyzing biofluids containing low levels of the model analytes.


Subject(s)
Antidepressive Agents, Tricyclic/blood , Antidepressive Agents, Tricyclic/urine , Body Fluids/chemistry , Liquid Phase Microextraction , Chromatography, Gas , Healthy Volunteers , Humans , Ions/blood , Ions/urine , Mass Spectrometry , Molecular Structure , Particle Size , Surface Properties
18.
Anal Chim Acta ; 1106: 52-60, 2020 Apr 15.
Article in English | MEDLINE | ID: mdl-32145855

ABSTRACT

This work describes a novel methodology to analyze four tricyclic antidepressants (amitriptyline, doxepin, imipramine and, nortriptyline) in urine samples by combining supramolecular microextraction and paper spray ionization mass spectrometry (PS-MS). The proposed method uses a supramolecular solvent in which reverse micelles of 1-decanol are dispersed in tetrahydrofuran (THF)/water. The extraction of the tricyclic antidepressants at pH 9.0 requires a sample volume of 10.0 mL, short extraction time (1.0 min of extraction and 5 min of centrifugation), low amounts of organic solvent (50 µL of 1-decanol and 200 µL of THF), and provides high preconcentration factors: 96.9 to amitriptyline, 93.6 to doxepin, 71.3 to imipramine, and 146.9 to nortriptyline. The quantification by PS-MS is fast and straightforward because chromatographic separation is not required and all analytes were determined simultaneously. The limits of detection (LOD), quantification (LOQ), and the precision (RSD, %) of the developed method ranged between 5.2 and 8.6 µg L-1, 17.4-28.7 µg L-1 and 1.3-12.9%, respectively. Urine samples of five individuals (three males and two females) were used for accuracy evaluation. The accuracy obtained in these spiked urine samples at µg L-1 levels varied from 95.3 to 112.0%. The method also provided clean mass spectra with a high signal-to-noise ratio, which demonstrates the analytical appeal combination of supramolecular microextraction with determination by paper spray mass spectrometry.


Subject(s)
Antidepressive Agents, Tricyclic/urine , Liquid Phase Microextraction , Paper , Amitriptyline/urine , Doxepin/urine , Humans , Imipramine/urine , Macromolecular Substances/chemistry , Mass Spectrometry , Molecular Structure , Nortriptyline/urine
19.
J Sep Sci ; 32(15-16): 2592-600, 2009 Aug.
Article in English | MEDLINE | ID: mdl-19606442

ABSTRACT

A poly(N-isopropylacrylamide-co-ethylene dimethacrylate) (poly(NIPAAm-co-EDMA)) monolith was in situ prepared in the capillary and was investigated for in-tube solid-phase microextraction (SPME). NIPAAm, an acrylamide monomer with isopropyl group, was crosslinked with EDMA. PEG of 400-20,000 Da molecular weight and methanol were selected as the binary porogens. The porous structures of the resulting monoliths have been assessed by SEM, nitrogen adsorption-desorption, and pressure drop measurements. To investigate the extraction mechanism, several groups of model analytes (including neutral, acidic, and basic) were examined. The result showed that this monolithic material exhibited high extraction efficiencies for compounds under highly acidic and basic conditions, which was due to the hydrophobic interactions and excellent pH stability of the monolith. The equilibrium extraction time profiles were also monitored for model compounds to evaluate the extraction capacity of monolithic capillary. Finally, the developed monolith in-tube SPME-HPLC method was applied to the determination of three tricyclic antidepressants from urine samples.


Subject(s)
Acrylamides/chemistry , Chromatography, High Pressure Liquid/instrumentation , Cross-Linking Reagents/chemistry , Methacrylates/chemistry , Solid Phase Microextraction/instrumentation , Antidepressive Agents, Tricyclic/isolation & purification , Antidepressive Agents, Tricyclic/urine , Chromatography, High Pressure Liquid/methods , Humans , Hydrogen-Ion Concentration , Molecular Weight , Polyethylene Glycols/chemistry , Porosity , Reproducibility of Results , Solid Phase Microextraction/methods
20.
Intern Med ; 58(18): 2627-2632, 2019.
Article in English | MEDLINE | ID: mdl-31527368

ABSTRACT

Objective In the management of patients with suspected acute drug poisoning, a screening test using the patient's urine is usually performed. The Triage DOA® and INSTANT-VIEW M-1® kits are two commonly used point-of-care screening kits in Japan. However, the relationship between the results of these screening kits and the blood concentration of the poisoning drug is not clear. In this study, we evaluated which kit is more useful for acute drug poisoning screening based on a comparison of their results with the results of a serum drug analysis. Methods This prospective cross-sectional study investigated all patients with acute drug poisoning admitted to a general hospital in Tokyo, Japan, over a nine-month period. The Triage DOA® and INSTANT-VIEW M-1® screening kits were used, and a qualitative serum analysis was conducted simultaneously in all cases. We compared the kits for use in screening patients with acute drug poisoning and evaluated the utility of the kits. Results For the 117 patients enrolled in this study, the 2 kits showed different sensitivities to benzodiazepines (Triage®, 78.6%; INSTANT-VIEW®, 90.5%). Both kits showed high sensitivity to barbiturates (Triage®, 87.0%; INSTANT-VIEW®, 91.3%) but low sensitivity to tricyclic antidepressants (Triage®, 25.0%; INSTANT-VIEW®, 45.8%). Conclusion Because the sensitivity varies depending on the kind of drug, it is difficult to discuss the superiority of these kits. However, this study compared the results of two types of urinary drug screening kits with the results of qualitative analysis of drugs in serum as a gold standard, providing important reference data.


Subject(s)
Mass Screening/methods , Reagent Kits, Diagnostic , Substance-Related Disorders/blood , Substance-Related Disorders/urine , Triage/methods , Adolescent , Adult , Aged , Aged, 80 and over , Antidepressive Agents, Tricyclic/blood , Antidepressive Agents, Tricyclic/urine , Barbiturates/blood , Barbiturates/urine , Benzodiazepines/blood , Benzodiazepines/urine , Cross-Sectional Studies , Female , Humans , Male , Middle Aged , Prospective Studies , Tokyo , Young Adult
SELECTION OF CITATIONS
SEARCH DETAIL