Determination Of Citalopram Research Articles

Determination of citalopram in fish brain tissue: benefits of coupling laser diode thermal desorption with low- and high-resolution mass spectrometry.

Recent state-of-the-art methods developed for the analysis of polar xenobiotics from different types of biological matrices usually employ liquid chromatography with mass spectrometry. However, there are limitations when a small amount of sample mass is available. For example, individual benthic invertebrates or fish tissue samples often weigh less than 100mg (e.g., brain, liver) but are necessary to understand environmental fate and bioaccumulation dynamics. We developed ultra-fast methods based on a direct sample introduction technique. This included coupling laser diode thermal desorption with atmospheric pressure chemical ionization mass spectrometry (LDTD-APCI-MS). We then quantitated a common selective serotonin reuptake inhibitor (citalopram) in brain tissues of individual juvenile fish after in vivo exposure to environmentally relevant concentration. Two mass spectrometric methods based on low (LDTD-APCI-triple quadrupole (QqQ)-MS/MS) and high (LDTD-APCI-high-resolution product scan (HRPS)) resolutions were developed and evaluated. Individual instrument conditions were optimized to achieve an accurate and robust analytical method with minimum sample preparation requirements. We achieved very good recovery (97-108%) across the range of 1-100ngg-1 for LDTD-APCI-HRPS. LDTD-APCI-QqQ-MS/MS showed poorer performance due to interferences from the matrix at the lowest concentration level. LDTD-APCI ionization was successfully validated for analysis of non-filtered sample extracts. Evaluation of final methods was performed for a set of real fish brain samples, including comparison of LDTD-APCI-HRPS with a previously validated LC-heated electrospray ionization-HRPS method. This new LDTD-APCI-HRPS method avoids the chromatographic step and provides important benefits such as analysis of limited sample masses, lower total sample volume (typically μL), and reduction in analysis time per sample run to a few seconds. Graphical abstract.

Development and validation of an ecofriendly chemiluminescence method for the determination of citalopram in pharmaceutical preparations using Cu2+-grafted Oxidized multiwall carbon nanotubes

Anovel and sensitive chemiluminescence (CL) method was developed and validated for the determination of citalopram in bulk dosage form and in pharmaceutical preparations. The method is based on the use of Cu 2+ -grafted oxidized multiwall carbon nanotubes (Cu/ox-MWCNTs). The weak CL signal arising fromthe reaction of an alkaline luminol-H 2 O 2 system was significantly enhanced by the addition of citalopram in the presence of ox-MWCNTs/Cu 2+ . Furthermore, ox-MWCNTs/Cu 2+ exhibited exceptional catalytic activity towards the oxidation of luminol in the luminol-H 2 O 2 CL reaction. Multiwalled carbon nanotubes (MWCNTs) were characterized by scanning electron microscopy (SEM), which also showed the attachment of Cu 2+ toMWCNTs. Various factors affecting CL intensity were carefully investigated and optimized for citalopram quantitation. The CL intensity was proportional to citalopram concentration in the range 0.2–8.0 μ g mL –1 , with a correlation coefficient of 0.996. The limit of detection (LOD) and limit of quantification were 2.29 × 10 –5 μ g mL –1 and 7.64 × 10 –5 μ g mL –1 , respectively, and its reproducibility was satisfactory with a relative standard deviation (RSD) of 2.59 % (n = 5). The interference effects of common excipients were studied, and the developed method was effectively applied for the determination of citalopram in pure formand in pharmaceutical preparations. Percentage recoveries were calculated and ranged from 98.67 to 101.46 % for the pure form and from 97.38 to 101.72 % for pharmaceutical preparations. Keywords: Chemiluminescence, Citalopram, Luminol, oxidized multiwall carbon nanotubes

Dendrimer-reinforced sol-gel based hollow fiber solid-phase microextraction for citalopram determination using response surface methodology.

The inclusion of a polyamidoamine dendrimer in a silica sol-gel yielded a solid nanosorbent that was used for the preconcentration, extraction, and determination of citalopram in hospital waste water, hemodialysis solution, and some drinking water. The method was developed by applying a novel nanosorbent for the solid-phase microextraction of citalopram, containing a silica sol-gel reinforced by polyamidoamine second-generation dendrimer, which was protected by a polypropylene hollow fiber. Plackett-Burman design and central composite design were utilized to evaluate the significance of several factors on the extraction efficiency. The adsorption mechanism and thermodynamic and kinetic aspects were studied. The adsorption process was exothermic and well fitted to the Bangham equation kinetic model. Under optimal conditions, the presented method was liner in the range of 0.05-100μg/mL. The limits of detection of quantification of citalopram were 0.0095 and 0.031μgm/L, respectively.

Application of ionic liquid-based ultrasonic-assisted microextraction coupled with HPLC for determination of citalopram and nortriptyline in human plasma

ABSTRACTIn this paper, an effective and environmentally friendly method of ultrasound-assisted ionic liquid-based dispersive liquid–liquid microextraction (UA-IL-DLLME) combined with high-performance liquid chromatography (HPLC)–photodiode array detector was applied for extraction and determination of two antidepressant drugs citalopram hydrobromide and nortriptyline hydrochloride from human plasma samples. Several important parameters affect the steps and efficiency of extraction, some of which are sample solution’s pH, type and volume of ionic liquid, ultrasonic time, centrifuging time and rate, and the ionic strength of solution. Optimum conditions were obtained at pH = 11, 1-octyl-3-methyl imidazolium hexafluorophosphate for ionic liquid, 55 µL for ionic liquid volume, 4 min for ultrasonic time, 5 min and 3,500 rpm for centrifuging time and rotation’s speed, due to ionic strength by the addition of NaCl 1%. Under optimized conditions, the linearity was obtained in the range of 0.02–2,000 µg/L, with correlation coefficients higher than 0.995. The limits of detection were 10 µg/L for citalopram and 6 µg/L for nortriptyline. Preconcentration factors were 920 for citalopram and 800 for nortriptyline. The present method of UA-IL-DLLME combined with HPLC was successfully used for the determination of citalopram and nortriptyline drugs in real samples of human plasma.

Optimization of ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplets by experimental design methodologies for determination of three anti-anxiety drugs in human serum and urine samples by high performance liquid chromatography

A novel coupling of ultrasound-assisted dispersive liquid–liquid microextraction based on solidification of floating organic droplets (UA-DLLME-SFODs) with high performance liquid chromatography (HPLC) was developed for the simultaneous preconcentration and determination of citalopram (CIT), diazepam (DIZ), and sertraline (SER) in their tablets and in the human serum and urine samples. In this proposed procedure, 1-undecanol and ethanol were used as the extraction and disperser solvents, respectively. Several parameters affecting the extraction efficiency were investigated using the Plackett–Burman (PB) factorial design as a screening design. The variables showing significant effects on the analytical response were the pH value for the sample solution and the volume of the extraction solvent; they were optimized using the central composite face-centered design (CCFD). For validation of the technique, its accuracy, precision, limit of detection (LOD), linearity, and sensitivity were evaluated. Also the limits of quantification (LOQs) were 1.3, 2.7, and 1.2ngmL−1 for CIT, DIZ, and SER, respectively. The extraction recovery percentages for all the examined drugs were above 92.9 with acceptable relative standard deviations (RSDs). The proposed methodology was successfully applied to the determination of these drugs in their tablets and in the human serum and urine samples.

A novel voltammetric sensor for citalopram based on multiwall carbon nanotube/(poly(p-aminobenzene sulfonic acid)/β-cyclodextrin)

Multi-walled carbon nanotube (MWCNTS) coated with poly p-aminobenzene sulfonic acid/β-cyclodextrin (p-ABSA/β-CD) film was used as an effective strategy for modification of the surface of glassy carbon electrode (GCE). Electrochemical study and determination of citalopram (CT) were investigated at the p (p-ABSA)/β-CD/MWCNT/GC using cyclic and differential pulse anodic stripping voltammetric techniques. The results indicate that the p (p-ABSA)/β-CD/MWCNT/GC significantly enhanced the oxidation peak current of CT. The modified electrode was characterized by electrochemical impedance spectroscopy (EIS), scanning electron microscopy(SEM) and cyclic voltammetry (CV).The fabricated electrochemical sensor exhibits a fast and reversible linear response toward CT within the concentration ranges of 90nM–1μM, 1–11μM and 11–100μM with correlation coefficients greater than 0.99 and detection limit of 44nM. The resulting functionalized polymer film features interesting electrochemical properties such good recovery, reproducibility and selectivity toward CT. The applicability of the proposed sensor was tested by determination of CT in pharmaceutical combinations and human body fluids.

Polypyrrole/magnetic nanoparticles composite as an efficient sorbent for dispersive micro-solid-phase extraction of antidepressant drugs from biological fluids

In this study, polypyrrole/magnetic nanoparticles composites in the presence of two different dopants were synthesized with the aid of chemical oxidative polymerization process for dispersive-μ-solid phase extraction (D-μ-SPE). The synthesized magnetic sorbents were characterized by various techniques. The results exhibited that the nanocomposite modified by polypyrrole with sodium perchlorate as a dopant demonstrated higher extraction efficiency for citalopram (CIT) and sertraline (STR) as the model compounds. This nanosorbent in combination with high performance liquid chromatography-UV detection was applied for extraction, preconcentration and determination of CIT and STR in urine and plasma samples. The effect of various parameters on the extraction efficiency including: sample pH, amount of sorbent, sorption time, eluent and its volume, salt content, and elution time were investigated and optimized. The opted conditions were: sample pH, 9.0; sorbent dosage, 10mg; sorption time, 7min; elution solvent and its volume, 0.06molL−1 HCl in methanol, 120μL; elution time, 2min and without addition of salt to the sample. The calibration curves were linear in the concentration range of 1–800μgL−1. The limits of detection (LODs) were obtained in the range of 0.2–1.0μgL−1 for CIT and 0.3–0.7μgL−1 for STR, respectively. The percent of extraction recoveries and relative standard deviations (n=5) were in the range of 93.4–99, 4.8–8.4 for CIT and 94–98.4, 4.3–9.2 for STR, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of CIT and STR in human urine and plasma samples.

HPLC Method for Chiral Separation and Quantification of Antidepressant Citalopram and Its Precursor Citadiol

HPLC method enabling chiral separation and determination of citalopram (CIT), a widely used antidepressant, and its synthetic precursor citadiol in one analysis was developed and validated. Moreover, supercritical fluid chromatography was also tested and was proved to be less effective for this separation purpose. The optimized HPLC system was composed of Chiralcel OD-H column and n-hexane/propane-2-ol/triethylamine 96/4/0.1 (v/v/v) as mobile phase, column temperature 25 °C, flow rate 1.0 mL min−1, UV detection at 250 nm. The effects of amount of propane-2-ol, triethylamine addition, and temperature on enantioselectivity and resolution of the enantiomers were evaluated. The method was found to be suitable for determination of the enantiomeric purity of CIT in bulk drugs. Enantiomers of CIT were determined in two commercially available pharmaceuticals.

Simultaneous Analysis of New Antidepressants by Densitometric Thin-Layer Chromatography

A simple and rapid TLC method using densitometric detection was developed for the simultaneous analysis of four SSRI antidepressants: citalopram, sertraline, fluoxetine, and fluvoxamine. The analytes were separated on silica gel 60 F254s TLC plates using a mobile phase composed of acetone-benzene-ammonia (50:45:5, v/v/v). Densitometric detection and quantification were carried out in the reflectance mode at 240 nm. The calibration curve was linear in the range of 500–5000 ng per spot for all analyzed compounds. The limit of detection was 40 ng per spot for citalopram and 50 ng per spot for fluoxetine, fluvoxamine, and sertraline, respectively. Statistical analysis proves that the method is both precise and accurate. The proposed method was successfully applied for the determination of citalopram and fluoxetine in their pharmaceutical formulations, with recoveries ranging from 98.7–101.9% of the labeled amount of the compounds. Finally, the reported method was also applied to the analysis of antidepressants in real biological samples.

Spectrofluorimetric method for determination of citalopram in bulk and pharmaceutical dosage forms

A simple accurate, sensitive reproducible spectrofluorimetric method was developed for the analysis of citalopram in pure and pharmaceutical dosage form. Citalopram showed strong native fluorescence in 0.05 M sulphuric acid having excitation at 239 nm and emission at 300 nm. All parameters like the effect of different solvents, pH, dilutions, reaction time, temperature and effect of excipients were thoroughly investigated. The calibration graph was linear in the range from 0.100 to 0.900 μg/ml. The proposed method was statistically validated and successfully applied for analysis of tablet dosage forms. The percentage recovery was found to be between 99.08% to 99.28%.

Development and Validation of Column High-Performance Liquid Chromatographic and Ultraviolet Spectrophotometric Methods for Citalopram in Tablets

Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30% triethylamine solution-acetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10% ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25 degrees C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.00-70.00 microg/mL, and 2.50-17.50 microg/mL for the UV spectrophotometric method. The interday and intraday assay precision was < 1.5% (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70-101.35% for the LC method and 98.48-98.65% for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.

Determination of citalopram and escitalopram together with their active main metabolites desmethyl(es-)citalopram in human serum by column-switching high performance liquid chromatography (HPLC) and spectrophotometric detection

We established a method for automated quantitative analysis of (es-)citalopram and desmethyl(es-)citalopram in serum using column-switching high performance liquid chromatography (HPLC). For sample clean-up serum was injected onto a LiChrospher CN 20 μm precolumn using 8% acetonitrile in deionized water. Drugs were eluted by back-flush flow onto the analytical column (LiChrospher CN 5 μm) at a flow rate of 1.5 ml/min with phosphate buffer 8 mmol/l pH 6.4/acetonitrile (50/50, v/v). Haloperidol was used as internal standard. Analytes were detected by ultraviolet spectrophotometry at 210 nm. Detection limit of (es-)citalopram was 6 ng/ml. The method was found to be suitable for therapeutic drug monitoring of patients treated with citalopram or escitalopram.

Capillary Electrophoretic Determination of Citalopram in Pharmaceutical Tablets and Serum

Determination of citalopram by capillary electrophoresis is described. Compounds were separated at 28 kV in 75 μm i.d. fused silica capillary tubing (total length 85 cm, effective length 65 cm) with 10 mM borate buffer, pH 8.5, containing 10% (v/v) methanol as running buffer. Citalopram and propylparaben (IS) appeared at 3.5 and 5.5 min, respectively. Repeatable linear results were obtained. The limits of detection and quantification were 5.73 × 10−6 and 1.72 × 10−5 M, respectively. When citalopram was determined in a pharmaceutical tablet by capillary electrophoresis and by a UV-spectrophotometric method differences between the results were not significant. The citalopram content of tablets was 100.8 ± 2.95% of the label claim. The amount found in serum was 26.7 ± 0.1% of the free drug, indicating that 73.3% of the drug was bound to protein.

Development and validation of a liquid chromatographic method for determination of enantiomeric purity of citalopram in bulk drugs and pharmaceuticals

A simple, rapid and robust LC method for enantiospecific separation and determination of citalopram in drugs and pharmaceuticals was developed using UV and polarimetric detectors connected in series. Baseline separation with resolution ≥ 3.0 was achieved within 20 min on Chiralcel OD-H (250 mm × 4.6 mm) 5 μm column using a mobile phase containing of n-hexane:2-propanol:triethylamine (TEA) (95:05:0.1 v/v/v) at a flow rate of 1.0 ml/min at 25 °C. Effects of 2-propanol, triethylamine and temperature on enantioselectivity and resolution of the enantiomers were evaluated. Clopidogrel hydrogen sulphate was used as an internal standard (IS) for quantitative determinations using UV detector at 240 nm. Polarimetric detector was used for identification of enantiomers. The limits of detection (LOD) and quantification (LOQ) were 0.5 and 1.3 μg/ml respectively for both the enantiomers. The linearity of the method was in the range of 50–600 μg/ml with r 2 > 0.9999. The inter- and intra-day assay precision was less than 0.63% (%R.S.D.) and recoveries were in the range 99.38–100.41%. The method was validated and found to be suitable for determination enantiomeric purity of citalopram in bulk drugs and pharmaceutical formulations.

Determination of Citalopram and its Main Metabolite Desmethylcitalopram in Human Serum by Column-Switching High Performance-Liquid Chromatography (HPLC) and Spectrophotometric Detection

Determination of Citalopram and its Main Metabolite Desmethylcitalopram in Human Serum by Column-Switching High Performance-Liquid Chromatography (HPLC) and Spectrophotometric Detection

High-performance liquid chromatographic determination of citalopram and four of its metabolites in plasma and urine samples from psychiatric patients

High-performance liquid chromatographic determination of citalopram and four of its metabolites in plasma and urine samples from psychiatric patients

Simultaneous determination of citalopram, monodesmethylcitalopram and didesmethylcitalopram in plasma by high-performance liquid chromatography after column extraction

Simultaneous determination of citalopram, monodesmethylcitalopram and didesmethylcitalopram in plasma by high-performance liquid chromatography after column extraction

Determination of citalopram in plasma and brain tissue of the rat by high-performance liquid chromatography with ultraviolet detection

Determination of citalopram in plasma and brain tissue of the rat by high-performance liquid chromatography with ultraviolet detection

Determination of citalopram, amitriptyline and clomipramine in plasma by reversed-phase high-performance liquid chromatography

The determination of citalopram, amitriptyline, clomipramine and their desmethyl metabolites after alkaline diethyl ether extraction from plasma is achieved by high-performance liquid chromatography using two internal standards and μBondapak C 18 as stationary phase. Elution is carried out isocratically at 0.5 or 1 ml/min with mixture of acetonitrile- potassium dihydrogen phosphate-distilled water (45:50:5). Detection is monitored by absorption at 254 nm. The detection limit is less than 5 ng/ml for each compound. The coefficients of variation are between 1.3% and 9.4% for 8-360 ng/ml. Interference from 22 possible co-medications is discussed. The technique can be used for therapeutic monitoring of these antidepressants as well as in analytical toxicology.