Determination Of Amitriptyline Research Articles

Magnetic Particle Spray Mass Spectrometry.

In this work, the concept of magnetic particle spray mass spectrometry (MPS-MS) is reported for the first time. Magnetic sorbent particles are used to extract the analytes from a liquid sample. The particles are magnetically attracted to the tip of a magnetic probe that is positioned at the entrance of the mass spectrometer. A solvent is dispensed on the particles, and a high voltage promotes the formation of the Taylor cone around the particles agglomerate. Analytes are desorbed by the solvent, ionized, and analyzed by mass spectrometry. MPS-MS is totally in consonance with the green chemistry principle. A minimal consumption of sample (100 μL), solvent (34 μL), and magnetic sorbent (500 μg) is needed per analysis for an excellent performance of MPS-MS in terms of sensitivity and selectivity. The determination of amitriptyline, citalopram, clomipramine, chlorpromazine, doxepin, haloperidol, nortriptyline, and venlafaxine in human plasma samples using magnetic restricted-access carbon nanotubes was carried out as a proof of principle. Limits of quantification of 10 μg L-1 and correlation coefficients higher than 0.98 were obtained for all of the analytes. Limits of detection ranged from 0.43 to 2.82 μg L-1. Precision (as relative standard deviation) and accuracies (as relative error) ranged from 3.6 to 23.6%, as well as -12.8 to 18.7%, respectively. MPS-MS opens a new line of developments in the association of sample preparation with ambient ionization. New sorbents, device configurations, and physical and chemical conditions can also be analyzed for the analysis of many other analytes in different samples.

Determination of Amitriptyline by Fluorescence Polarization Immunoassay

Determination of Amitriptyline by Fluorescence Polarization Immunoassay

Nanoscale materials in the composition of biosensors for the determination of amitriptyline

Biosensor devices including hybrid nanostructures as modifiers of transducer surfaces meet current requirements for the methods of research and determination of drugs, including antidepressants. The fea­tures of amperometric monoamine oxidase biosensors based on printed carbon electrodes modified with nanocomposite compositions C60 / cobalt nanoparticles/amino derivative of polyether polyol of the second generation/chitosan nanocomposite structures used for the detection of tricyclic antidepressant amitriptyline are considered. The choice of the best modifier was made proceeding from the data of transmission electron microscopy, scanning electron microscopy, electrochemical impedance spectroscopy, and differential pulse voltammetry. When developing the biosensor, conditions for depositing the composite composition of cobalt nanoparticles/amino derivative of polyether polyol on the electrode surface were varied: electrochemical deposition, sequential layer-by-layer deposition, and deposition of the mixture. The peak of electrochemical oxidation of hydrogen peroxide, which is formed during the enzymatic reaction of serotonin oxidation under the action of monoamine oxidase was used as an analytical signal of the biosensor. The principle of the biosensor action is based on the inhibitory effect of amitriptyline on the catalytic activity of immobilized monoamine oxidase. The proper choice of a modifier and optimal working conditions provided the range of detectable concentrations of amitriptyline: 1 x 10-4 - 1 x 10-8 M, the lower limit of the determined content at a level of 5 x 10-9 M for monoamine oxidase biosensor. Comparison of the results on the amitriptyline content determination in the pharmaceutical preparation and urine obtained using the monoamine oxidase biosensor and polarization fluorescence immunoassay (dilution of the tracer 1:32, dilution of antibodies 1:128, the range of working concentrations 5 x 10 -8 — 5 x 10-9 M), well-proven in the quantitative determination of medicinal substance, confirmed the correctness of the results obtained.

Electrocatalytic Behavior and Determination of Amitriptyline Drug with MWCNT@Celllulose Composite Modified Glassy Carbon Electrode.

A novel nanocomposite of cellulose based on multiwalled carbon nanotube (MWCNT) was synthesized by a simple solution mixing–evaporation method. The morphology, thermal investigations, electrocatalytic oxidation of amitriptyline were analyzed at multi-walled carbon/cellulose nanocomposite in detail. The amitriptyline (AMT) drug was electrochemically studied in a phosphate buffer at different pH using the MWCNT/cellulose modified glassy carbon electrode (GCE). As per the linear relationship among AMT along with peak current, differential pulse voltammetry technique has been established for their quantitative pharmaceutical’s determination. The oxidation potential shifted negatively compared to GCE, showing that the MWCNT/cellulose modified electrode had an excellent catalytic activity for the AMT oxidation. The anodic peak current varied linear response with AMT’s concentration in the range of 0.5 to 20.0 μM with a LOD of 0.0845 μM and LOQ of 0.282 μM, respectively. The proposed method was effectively put on the determination of AMT in pharmaceutical and urine samples. This novel methodology is presented here as an example of a complete development methodology for the determination of amitriptyline drug and sensor for use in healthcare fields.

Hybrid Nanocomposites as Electrode Modifiers in Amperometric Immunosensors for the Determination of Amitriptyline

Various nanostructured materials (graphene, fullerene C60, carbon nanotubes, and cobalt nanoparticles as a label) are used as nanocomposites to modify the surface of primary signal converters (screen-printed graphite electrode) in the development of amperometric immunosensors for the determination of tricyclic antidepressant amitriptyline. The use of nanomaterials improved the analytical characteristics of the corresponding immunosensors. The range of working concentrations of the immunosensor is 1 × 10–9–1 × 10–4 M, the lower limit of the analytical range is at a level of 5 × 10–10 M. The binding constants of antigen–antibody immune complexes are determined. Immunosensors are tested in the control of contents of medicinal preparations in urine.

Preparation and evaluation of magnetic core–shell mesoporous molecularly imprinted polymers for selective adsorption of amitriptyline in biological samples

Abstract In this study, preparation of magnetic surface molecular imprinted polymer (MMIP) is employed for sensitive solid phase extraction and measurement of amitriptyline (AMT) by spectrophotometric technique. After polymerization, cavities in the polymer particles corresponding to the AMT were created by leaching the polymer by an appropriate solution. The synthesized nanoparticles of magnetic surface molecular imprinted polymer mesoparticles (Fe3O4@SiO2–MIP) were characterized by transfer electron microscopy (TEM), vibrating sample magnetometer (VSM), Fourier transform infrared spectroscopy (FTIR), X-Ray Diffraction (XRD) and Brunauer–Emmett–Teller (BET). Also, the pH of zero-point charge (pHzpc) for Fe3O4@SiO2–MIP was determined with the pH drift method. The influence of various parameters such as pH, amount of polymer and contact time were investigated by an optimization technique named Box–Behnken design (BBD) and the proposed quadratic model was fitted very well with the experimental data. The validity of optimum parameters and the equation of parameters were investigated by analysis of variance (ANOVA). Also Scatchard isotherm was explored for the equilibrium adsorption investigation and finally, the prepared polymer was successfully applied to the selective identification and the determination of AMT in plasma samples.

A new effective on chip electromembrane extraction coupled with high performance liquid chromatography for enhancement of extraction efficiency

In the present research, an effective on chip electromembrane extraction (CEME) coupled with high performance liquid chromatography was presented for analysis of nortriptyline (NOR) and amitriptyline (AMI) as basic model analytes from urine samples. The chip consists of two polymethyl methacrylate (PMMA) parts with two craved microfluidic channels in each part. These channels were used as flow path for the sample solution and a thin compartment for the acceptor phase. A porous polypropylene sheet membrane impregnated with an organic solvent was placed between two parts of chip device to separate the channels. Two platinum electrodes were mounted at the bottom of these channels that were connected to a power supply providing the electrical driving force for migration of ionized analytes from sample solution through the porous sheet membrane into the acceptor phase. This new setup provides effective and reproducible extractions with low volume of sample solution. Efficient parameters on CEME of the model analytes were optimized using one variable at a time method. Under the optimized conditions, the calibration curve was linear in the range of 10.0–500 μg L−1 with coefficient of determination (r2) more than 0.9902. The relative standard deviations (RSDs %) for extraction and determination of the analytes were less than 6.8% based on six replicate measurements. LODs less than 4.0 μg L−1 were obtained for both of the model analytes. The preconcentration factors higher than 17.0-fold were obtained. The results demonstrated that CEME would be used efficiently for extraction and determination of AMI and NOR from urine samples.

Development and validation of a densitometric-high-performance thin-layer chromatographic method for quantitative analysis of amitriptyline in gastric lavage

Drug overdose is the most common method in suicide attempts. Amitriptyline (AMT), a tricyclic antidepressant agent, known for potentially lethal cardiovascular and neurological effects, is used especially by intoxicated patients. The aim of this study was to validate a method for the determination of AMT in gastric lavage samples by high-performance thin-layer chromatography (HPTLC). Artificial gastric lavage was used to obtain a better extraction procedure for AMT. The method was also applied to patients who attempted suicide with AMT. A validated, accurate, and rapid HPTLC-based method was developed for quantitation of AMT in gastric content of intoxicated patients. Extraction was done from 3 mL gastric lavage sample by liquid-liquid extraction procedure with ethyl acetate-n-heptane (1:1, w/w) in alkaline pH with 10.8. The mobile phase was an isocratic solvent system consisting of methanol-ammonia (25%) (98.5:1.5, v/v). 3,4-Methylenedioxy-Nmethamphetamine (MDMA) was used as internal standard (IS). Analy...

New HPLC method to detect amitriptyline in the blood of rats on combination treatment

Abstract A rapid, sensitive and specific method based on high performance liquid chromatography (HPLC) has been developed for the simultaneous determination of amitriptyline hydrochloride and Sildenafil citrate in the blood of rats. Sample preparation involved liquid–liquid extraction with n-hexane after alkalified with 0.5 M NaOH. Chromatographic separation was performed on XDB C-18 column with particle size of 5 μm (150 × 4.6 mm) with mobile phase acetonitrile and 20 mM KH 2 PO 4 buffer, pH = 3 using flow rate 1.5 ml/min. Calibration curves were linear within the ranges of 0.25–50 and 0.1–50 μg/ml for amitriptyline hydrochloride and Sildenafil citrate, respectively. This method was successfully applied to the pharmacokinetic study in rats after oral administration of amitriptyline hydrochloride and Sildenafil citrate for 24 h.

Simple, Rapid and Sensitive UV-Visible Spectrophotometric Method for Determination of Antidepressant Amitriptyline in Pharmaceutical Dosage Forms

The paper describes a new and simple approach for spectrophotometric determination of tricyclic antidepressant drug amitriptyline. Enhancement of the colour intensity of the Fe(III)-SCN−complex on addition of the drug amitriptyline forms the basis of the proposed method. The value of molar absorptivity of the Fe(III)-SCN−amitriptyline ion pair complex in terms of the drug lies in the range of (2.82–3.36) × 103 L·mol−1·cm−1at the absorption maximum 460 nm. The detection limit of the method was 0.3 μg·mL−1. The slope, intercept, and correlation coefficients for the present method were found to be 0.008, 0.002, and +0.998, respectively. The effect of analytical variables on the determination of the drug and the composition of the complex are discussed in the paper. The method is applicable in the determination of amitriptyline in pharmaceutical preparations.

New Approach for the Determination of Tricyclic Antidepressant Amitriptyline Using <i>β</i>-Cyclodextrin-PEG System via Spectrophotomerty

A new and simple procedure for the spectrophotometric determination of the tricyclic antidepressant drug amitriptyline is proposed. The method is based on enhancement of sensitivity of the [AMIYTP]+ β-cyclodextrin and PEG molecules involved in formation of molecules inclusion complex, in presence of polyethylene glycol (PEG) medium. The mole ratio of [AMIYTP]+ β-cyclodextrin and PEG molecules in inclusion complex were determined by the curve fitting method. The value of molar absorptivity of {[AMIYTP: (β CD)] PEG} complex in term of the drug lies in rage of (2.20 - 2.23) × 104 L·mole–1·cm–1 at absorption maximum 242 nm. The slope, intercept and correlation co-efficient were found to be 14.21, 0.0046, and 0.998, respectively. The effect of analytical variables on the determination of the drug and composition of the ion associated complex are discussed in the paper. This method is applicable in the determina-tion of amitriptyline in the pharmaceutical preparations.

Separation and Determination of Amitriptyline and Nortriptyline in Biological Samples Using Single-Drop Microextraction with GC

The combination of liquid phase microextraction (LPME) based on a single drop and gas chromatography flame ionization detector (GC-FID) was used for separation and determination of amitriptyline and nortriptyline in human plasma and urine samples. The sample solution was kept alkaline (pH 12), then a microdrop of organic solvent (isooctane) was suspended in the donor solution; after extraction, the organic microdrop was injected into the GC-FID. Experimental LPME conditions were optimized. Finally, the enrichment factors (89.5–139.0), the relative standard deviation (RSD%, n = 5) 1.1–8.5, linearity ranges (0.05–20 μg mL−1), and the limits of detections (0.01, 0.02 μg mL−1) for selected drugs were evaluated.

Simultaneous Spectrophotometric Determination of Amitriptyline Hydrochloride and Chlordiazepoxide in Pharmaceutical Tablets by Multivariate Calibration Method

The multivariate calibration method, partial least square regression (PLS) was applied for the simultaneous spectrophotometry determination of amitriptyline hydrochloride (AMT) and chlordiazepoxide (CHL) in their mixtures. The parameters of chemometric technique were optimized and the proposed method was validated with synthetic samples and applied to analyze these drugs in pharmaceutical products with good accuracy and precision. The results were compared with those given by United State Pharmacopoeia method. The square of the correlation coefficients (R2) for predicted AMT and CHL with the proposed method in a test sample were 0.9951 and 0.9897 respectively. The relative standard deviation for commercial tablets in the proposed method and USP standard method were 0.42 and 2.61%, respectively.

Separation and determination of amitriptyline and nortriptyline by dispersive liquid–liquid microextraction combined with gas chromatography flame ionization detection

Dispersive liquid–liquid microextraction (DLLME) coupled with gas chromatography–flame ionization detection (GC–FID) was applied for the determination of two tricyclic antidepressant drugs (TCAs), amitriptyline and nortriptyline, from water samples. This method is a very simple and rapid method for the extraction and preconcentration of these drugs from environmental sample solutions. In this method, the appropriate mixture of extraction solvent (18 μL Carbon tetrachloride) and disperser solvent (1 mL methanol) are injected rapidly into the aqueous sample (5.0 mL) by syringe. Therefore, cloudy solution is formed. In fact, it is consisted of fine particles of extraction solvent which is dispersed entirely into aqueous phase. The mixture was centrifuged and the extraction solvent is sedimented on the bottom of the conical test tube. 2.0 μL of the sedimented phase is injected into the GC for separation and determination of TCAs. Some important parameters, such as kind of extraction and disperser solvent and volume of them, extraction time, pH and ionic strength of the aqueous feed solution were optimized. Under the optimal conditions, the enrichment factors and extraction recoveries were between 740.04–1000.25 and 54.76–74.02%, respectively. The linear range was (0.005–16 μg mL −1) and limits of detection were between 0.005 and 0.01 μg mL −1 for each of the analytes. The relative standard deviations (R.S.D.) for 4 μg mL −1 of TCAs in water were in the range of 5.6–6.4 ( n = 6). The performance of the proposed technique was evaluated for determination of TCAs in blood plasma.

SPECTROPHOTOMETRIC DETERMINATION OF SOME ANTIDEPRESSANT DRUGS

ABSTRACT Amitriptyline and desipramine hydrochlorides react with niobium (V) thiocyanate complex forming yellow ion-association compounds. These compounds are insoluble in water, but fairly soluble in organic solvents. The formation and extraction conditions of the compounds have been established, and a new spectrophotometric method has been developed for the determination of amitriptyline and desipramine in the concentration range of 1–12 µg/mL and 1–6 µg/mL, respectively.

Determination of amitriptyline and nortriptyline in spiked plasma by capillary zone electrophoresis with β-cyclodextrin

A simple capillary zone electrophoresis (CZE) method was developed for the simultaneous analysis of amitriptyline (AMI) and its active metabolite (nortriptyline, NOR) in human plasma. This method was performed by Tris buffer (20 mM, pH 3.0) in the presence of β-cyclodextrin (0.2 mM). Several parameters affecting the separation of AMI and NOR such as the type and concentration of cyclodextrin, pH and concentration of Tris buffer were studied. Application of the method to the analysis of AMI and NOR spiked in plasma was conducted using clomipramine (CLO, 1 nmol) as an internal standard. After liquid–liquid extraction and concentration of AMI and NOR from plasma, the resulting residue was dissolved in aqueous acid prior to their analysis by capillary electrophoresis using UV detection (200 nm). In spiked plasma (1 ml) the quantitative ranges were 160–630 ng for AMI and 150–600 ng for NOR. The intra- and inter-day relative standard deviation ( n=3) were all less than 10% for each substance. The detection limits for plasma samples were found to be about 60 ng/ml for AMI and 70 ng/ml for NOR ( S/ N=3, injection 20 s). All recoveries for AMI and NOR were greater than 80%.

Application of Thiocyanate Complex of Titanium (IV) to the Extractive Spectrophotometric Determination of Amitriptyline Hydrochloride

Amitriptyline hydrochloride reacts in acidic medium with the thiocyanate complex of titanium (IV) forming a yellow ion- association compound, insoluble in water but fairly soluble in a mixture of chloroform and butyl alcohol (4:1). The formation and extraction conditions of the compound are described. The compound was characterized by UV, VIS, IR and 1H NMR spectrometry. The colored compound exhibits a maximum absorption at 360 nm. Under the optimum experimental conditions, amitriptyline hydrochloride was determined in the 3-60 μg/cm3 range with a relative standard deviation less than 0.5% (n=8). The proposed method was verified against the pharmacopoeial method and applied to the determination of amitriptyline hydrochloride in pharmaceuticals.

Solid-Phase Extraction for the Determination of Tricyclic Antidepressants in Serum Using a Novel Polymeric Extraction Sorbent

A fast and easy solid-phase extraction method was developed for the determination of amitriptyline, doxepin and their metabolites (nortriptyline and nordoxepin) in porcine serum matrix by high performance liquid chromatography. The spiked serum sample was pretreated with 2% phosphoric acid followed by a simple and rugged SPE procedure using OasisTM HLB extraction cartridges. The SPE method requires only one mL of simple solvent throughout the entire SPE process. High and reproducible recoveries were obtained even though the cartridges ran dry. For five replicate analyses, the average recoveries of parent tricyclic antidepressants and their metabolites were all greater than 94%, and the RSDs were all less than 4.0%.

Solid-Phase Extraction and High Performance Liquid Chromatographic Determination of Amitriptyline and Nortriptyline in Human Plasma

A simple, rapid, cost-efficient solid-phase extraction and high performance liquid chromatographic method for the determination of amitriptyline and nortriptyline in human plasma is described. After conditioning of solid-phase sorbent diluted plasma samples were passed through the cartridge. Potentially interfering substances were washed, followed by elution of amitriptyline, nortriptyline and maprotiline (internal standard) from the sorbent. Eluates were collected, evaporated, reconstituted and injected directly and monitored at 215 nm. Samples were chromatographed on a 5 μm Supelcosil LC-PCN (150 × 4.6 mm) using 0.01 M dipotassium hydrogenphosphate (pH adjusted to 7 with 85% ortophosphoric acid)/ acetonitrile/methanol (15:60:25. v/v) as the mobile phase. Recoveries for amitriptyline and nortriptyline were 96% and 85%, respectively. The limit of detection and quantification for amitriptyline and nortriptyline were 1 ng/mL and 5 ng/mL, respectively. The calibration curves for amitriptyline and nortriptyline in human plasma were linear over the range 5–500 ng/mL. The method was applied in single dose (75 mg) clinical pharmacokinetic studies of amitriptyline in depressed patients.

A Modified Simple and Rapid Reversed Phase High Performance Liquid Chromatographic Method for Quantification of Amitriptyline and Nortriptyline in Plasma

Abstract A simple and rapid reversed-phase liquid chromatographic method for the determination of amitriptyline and nortriptyline in plasma is described. Protriptyline was used as internal standard. Plasma samples were extracted from alkaline pH with hexane-isoamylalcohol 98:2 v/v for 60 sec on a vortex apparatus. The organic phase was back extracted with HCl 0.1N and the aqueous phase was injected directly and monitored at 240nm. Samples were chromatographed on a 5 μm Kromasil 100-C8 column (25 cm × 4 mm i.d) using acetonitrile/0.04M KH2PO4 40:60 v/v as the mobile phase. The lower limit of detection was 5 ng/ml for amitriptyline and nortriptyline while the lower limit of quantification was 10 ng/ml for both compounds. Peak height and plasma amitriptyline or nortriptyline concentrations were linearly related from 25 to 300 ng/ml. No potential sources of interference have been identified. The methodology was used to monitor plasma amitriptyline or nortriptyline concentrations in patients receiving therapeu...