Determination Of N-acetylcysteine Research Articles

Determination of N-Acetylcysteine in Pure and Drug Formulations Using Inhibitory Kinetic Approach

Determination of N-Acetylcysteine in Pure and Drug Formulations Using Inhibitory Kinetic Approach

P23 | Determination of N‐acetylcysteine in chicken plasma by LC–MS/MS analysis

Journal of Veterinary Pharmacology and TherapeuticsVolume 46, Issue S1 p. 96-97 POSTER PRESENTATIONS P23 | Determination of N-acetylcysteine in chicken plasma by LC–MS/MS analysis First published: 11 June 2023 https://doi.org/10.1111/jvp.13302Read the full textAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL No abstract is available for this article. Volume46, IssueS1Special Issue: 15th International Congress of the European Association for Veterinary Pharmacology and Toxicology held Bruges, Belgium, July 2–5, 2023June 2023Pages 96-97 RelatedInformation

Electro-catalytic amplified sensor for determination of N-acetylcysteine in the presence of theophylline confirmed by experimental coupled theoretical investigation

The 1,l/-bis(2-phenylethan-1-ol)ferrocene, 1-butyl-3-methylimidazolium hexafluoro phosphate (BMPF6) and NiO-SWCNTs were used to modify carbon paste electrode (BPOFc/BMPF6/NiO-SWCNTs/CPE), which could act as an electro-catalytic tool for the analysis of N-acetylcysteine in this work. The BPOFc/BMPF6/NiO-SWCNTs/CPE with high electrical conductivity showed two completely separate signals with oxidation potentials of 432 and 970 mV for the first time that is sufficient for the determination of N-acetylcysteine in the presence of theophylline. The BPOFc/BMPF6/NiO-SWCNTs/CPE showed linear dynamic ranges of 0.02–300.0 μM and 1.0–350.0 μM with the detection limit of ~ 8.0 nM and 0.6 μM for the measurement of N-acetylcysteine and theophylline, respectively. In the second part, understanding the nature of interaction, quantum conductance modulation, electronic properties, charge density, and adsorption behavior of N-acetylcysteine on NiO–SWCNTs surface from first-principle studies through the use of theoretical investigation is vital for designing high-performance sensor materials. The N-acetylcysteine molecule was chemisorbed on the NiO–SWCNTs surface by suitable adsorption energies (− 1.102 to − 5.042 eV) and reasonable charge transfer between N-acetylcysteine and NiO–SWCNTs.

Determination of N-acetylcysteine in the presence of ciprofloxacin or levofloxacinin microparticulate dry powder inhalers

A fast and easy method was validated for simultaneous determination of ciprofloxacin hydrochloride monohydrate (CP), levofloxacin hemihydrate (LV), and N-acetylcysteine (NAC) in samples. The analysis was performed on a C$_{18}$ column (250 x 4.6 mm, 5 μm) (Inertsil ODS-3V) using an isocratic elution method with a mobile phase composed of 25 mM KH$_{2}$PO$_{4}$ (pH 3.0) and methanol (72:28, v/v) at a flow rate of 1 mL/min. UV detection was performed at 214 nm for NAC and 293 nm for CP and LV. The method was validated for linearity, accuracy, precision (repeatability and reproducibility), specificity, sensitivity, and stability. The calibration study using several media demonstrated that the calibration curves were linear for all compounds in all media (R$^{2}$ > 0.9993). The limit of detection was 0.098 μg/mL for CP, 0.049 μg/mL for LV, and 0.487 μg/mL for NAC. The limit of quantification was 0.328 μg/mL for CP, 0.165 μg/mL for LV, and 1.624 μg/mL for NAC. Precision and accuracy values of the method fulfilled the required limits. All these outcomes demonstrate that the validated HPLC method is appropriate for simultaneous analysis of CP, LV, and NAC in samples for content uniformity of dry powder inhaler and permeability studies.

Poly(adenine) DNA-Templated Gold Nanocluster-Based Fluorescent Strategy for the Determination of Thiol-Containing Pharmaceuticals

The fluorescence intensity of poly(adenine) DNA-templated gold nanoclusters was shown to be significantly quenched by N-acetylcysteine through the formation of the Au-S metal-ligand bonds. On the basis of the fluorescence quenching phenomenon, a sensitive, turn-off, and label-free fluorescence method has been designed for the determination of thiol-containing pharmaceuticals using poly(adenine) DNA-templated gold nanoclusters as fluorescent probes. The assay exhibited sensitive determination of N-acetylcysteine with a linear dynamic range from 10 nM to 10 μM and a limit of detection of 3 nM. Furthermore, the proposed strategy was successfully applied for the determination of N-acetylcysteine levels in acetylcysteine granule samples. Thus, the method could provide a sensitive, simple, and rapid fluorescent sensing platform for the determination of thiol-containing pharmaceuticals.

Simultaneous Determination of N-Acetyl Cysteine and Taurine by HPTLC Method in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form

Specific, precise and sensitive TLC-Densitometric method was developed and validated for the simultaneous estimation of N-Acetyl cysteine and Taurine in active pharmaceutical ingredient and pharmaceutical dosage form. An effective separation was achieved on pre-coated silica gel HPTLC plates by using n-butanol:acetic acid:water (8:0.5:1.5 v/v/v). The spots were scanned densitometrically at 295 nm. The RF values of N-Acetyl cysteine and Taurine were found to be 0.29 and 0.52, respectively. Calibration curves were linear in the range of 30 - 180 and 100 - 600 ng/band for N-Acetyl cysteine and Taurine, correspondingly with correlation coefficients of 0.999. The developed method was validated as per ICH guidelines. The limits of detection were 11.24 and 63.40 ng/spot for NAC and TAU respectively. The method developed was found to be precise and specific for the simultaneous analysis of N-Acetyl cysteine and Taurine in pure and tablet dosage form.

Toxicity Patterns and Outcomes in Acute Acetaminophen Ingestions

Objective: Core idea of this research is to comprehend acute acetaminophen toxicities, towards the determination of N-Acetyl Cysteine, relevant time of onset added by protocol therapy. It also looks into determined outcomes. Subjects and methods: In current research followed retrospective plan of study with a level of eligibility of 307 patients (among whom 200 are males and 107 are females). These patients were from all the age groups and were suffering from acute acetaminophen toxicities as noted within October 2010 to the month of September 2012. These people also have ingestion acetaminophen through intentional/unintentional aspects, and the level of serum acetaminophen under detectable level. Results: Poisoned acetaminophen offers determined percentage as per ER visits of 307 poisoning case within 1884 (that is 16.2%). Just 6.2% of entire acetaminophen toxicities offered possible/probable hepatic toxicities added by NAC as prescribed with nearly noted equal distribution made through intentional as well as unintentional poisoning mode (52.7% or 47.3%). Conclusions: There is complete recovery without any mortality record being featured in current research attributing towards very low chronic alcoholism instances as in relevant case studies.

A GREEN HPLC METHOD FOR THE DETERMINATION OF N-ACETYLCYSTEINE USING POST-COLUMN DERIVATIZATION WITH METHYL-PROPIOLATE

In this study, a new, green analytical method is proposed for the determination of N-acetylcysteine (NAC) in pharmaceutical formulations. The analyte was separated from the samples matrix using a 100% aqueous mobile phase [0.05% v/v CH3COOH+1 mmol L−1 ethylenediaminetetraacetic acid (EDTA) in water] and a suitable analytical column (Prevail reversed phase column). Detection was carried out at 285nm after on-line post-column derivatization (PCD) with methyl-propiolate (MP) in alkaline medium. Method development included both chromatographic and reaction parameters, while validation was based on international recommendations. The developed analytical scheme excludes the use of organic modifiers from all steps of pretreatment/analysis and offers adequate figures of merit for the quality control (assay and content uniformity) of NAC-containing formulations.

Modified multiwalled carbon nanotubes paste electrode as a sensor for the electrocatalytic determination of N-acetylcysteine in the presence of high concentrations of folic acid

A new vinylferrocene modified-multiwalled carbon nanotubes paste electrode was prepared and used for the determination of N-acetylcysteine (N-AC) and folic acid (FA). Using the modified electrode, a highly selective square wave voltammetric method for the simultaneous determination of N-AC and FA was developed. The peak currents of N-AC and FA increased linearly with their concentration in the ranges of 0.1–662 and 10.0–900 μmol L−1, respectively, with corresponding detection limits of 0.09 and 7.0 μmol L−1. The RSD% for 0.7 μmol L−1N-AC was 1.5%, whereas for 15.0 μmol L−1 FA, it was 1.9%. Well separated oxidation peaks of N-AC and FA were obtained at pH 7.0 with this modified electrode. The modified electrode was successfully applied for the simultaneous determination of N-AC plus FA in real samples.

Flow Injection Spectrophotometric Determination of N-Acetylcysteine and Captopril Employing Prussian Blue Generation Reaction

A novel flow injection procedure to determine N-acetylcysteine and captopril in pharmaceutical formulations is proposed. The flow procedure developed was based on oxidation of the analytes by Fe(III) in acidic medium and subsequent reaction of the Fe(II) generated with excess hexacyanoferrate(III) to produce soluble Prussian blue (KFe[Fe(CN)6]) measured at 700 nm. Detection limits of 1.0 × 10−5 mol L−1 and 3.0 × 10−5 mol L−1 for N-acetylcysteine and captopril, respectively, were found. The sample throughput was 70 h−1 for both analytes and the results obtained were in agreement at a 95% confidence level with those obtained using reference methods.

Determination of N-Acetylcysteine by Cyclic Voltammetry Using Modified Carbon Paste Electrode with Copper Nitroprusside Adsorbed on the 3–Aminopropylsilica.

Determination of N-Acetylcysteine by Cyclic Voltammetry Using Modified Carbon Paste Electrode with Copper Nitroprusside Adsorbed on the 3–Aminopropylsilica.

On-Line Derivatization of N-acetylcysteine Using Ethyl-Propiolate as a Novel Advantageous Reagent and Sequential Injection Analysis

This study reports a novel automated assay for the determination of N-acetylcysteine (NAC). The method is based upon the on-line derivatization of the analyte with a new reagent, ethyl-propiolate (EPL), to form a UV-absorbing derivative. The reaction is fast, proceeds in aqueous solutions under mild conditions and is, therefore, ideal for automation using sequential injection analysis. All major chemical and instrumental variables were examined thoroughly. The assay was validated for linearity, range, LOD-LOQ, within and day-to-day precision, selectivity, and accuracy. The experiments confirmed its suitability for the reliable quality control of NAC-containing formulations at a sampling rate of 80 h−1.

Determination of N-Acetylcysteine and Main Endogenous Thiols in Human Plasma by HPLC with Ultraviolet Detection in the Form of Their S-Quinolinium Derivatives

A new, sensitive, repeatable, and robust high performance liquid chromatography assay for the determination of total N-acetylcysteine, cysteine, cysteinylglycine, glutathione, and homocysteine in human plasma has been developed. The thiol concentrations were measured using precolumn specific derivatization with 2-chloro-1-methylquinolinium tetrafluoroborate, followed by high performance liquid chromatographic reversed phase separation with spectrophotometric detection. The oxidized and protein bound forms of thiols were converted into their reduced forms employing a reductive agent tris(2-carboxyethyl)phosphine. The chromatographic separation was accomplished in 12.5 min; the within run and between run imprecision were all less than 10%. The elution profile was as follows: 0–4 min, 11% B; 4–8 min, 11–30% B; 8–12 min, 30–11% B. The calibration graphs, obtained with the use of normal plasma spiked with growing amounts of analytes, were linear over the concentration ranges, covering most experimental and clinical cases (1–32 µM for homocysteine and glutathione, 1–320 µM for N-acetylcysteine and cysteine, and 1–64 µM for cysteinylglycine). For all analytes, recoveries between 91.2 and 108.6%, were observed.

Determination of N-Acetylcysteine and Thioglycolic Acid in Human Urine

A method for the determination of total N-acetylcysteine and thioglycolic acid in human urine is described. Because these compounds are mainly excreted as disulfides, they are first reduced to the free thiols by treatment with tris(2-carboxyethyl)phosphine hydrochloride and then derivatized with 2-chloro-1-methylquinolinium tetrafluoroborate. Separation and quantitation of the 2-S-quinolinium derivatives of the thiols were achieved by reversed-phase ion-pair liquid chromatography with UV-detection at 355 nm. Because the method enables simultaneous determination of other endogenous urinary thiols, e.g. cysteine and cysteinylglycine, amounts of these compounds in urine were also studied. Detector responses were linear over the range covering most practical situations, with correlation coefficients for all four analytes better than 0.999. Recovery and imprecision (as RSD) were within 99.77–102.17 and 0.01–7.79%, respectively. The lower limit of detection was 0.25 μmol L−1 urine for thioglycolic acid and N-acetylcysteine, and 0.12 μmol L−1 urine for cysteine and cysteinylglycine. The method was used for analysis of urine samples from 29 healthy individuals to establish reference values for the thiols, normalized to creatinine. 3-Mercaptolactic acid, 2-mercaptopropionic acid, and mercaptoethanol were not present in the urine analyzed.

Determination of N-acetylcysteine in human plasma by liquid chromatography coupled to tandem mass spectrometry

An analytical method for the determination of total N-acetylcysteine in human plasma has been developed, validated and applied to the analysis of samples from a phase I clinical trial. The analytical method consists of plasma digestion with dithiothreitol in order to reduce all the oxidized forms of N-acetylcysteine, and extraction with ethyl acetate followed by determination of levels by an LC–MS–MS method. The intra- and inter-assay precision and accuracy of this technique were good and the limit of quantitation was 50 ng/ml of plasma. The concentration working range was established between 50 ng/ml and 1000 ng/ml. This method has been used in the analysis of approximately 800 human plasma samples from a clinical study with 24 volunteers; the precision of the quality controls was in the range 8.7 to 13.4% and the accuracy was in the range −5.9 to 8.5%, expressed as the RSD and the relative error, respectively.

Determination of N-acetylcysteine in pharmaceutical samples by flow injection

Two flow injection (FI) methods, involving spectrophotometric detection, are proposed for the determination of N-acetylcysteine (NAC). Both methods are based on the formation of a yellow complex between NAC and PdII in a medium of 1 mol dm–3 HCl. In the first method, which is based on the conventional Fl technique, NAC is determined over the range 5 × 10–5–5 × 10–3 mol dm–3, and in the second, in which the doublet-peak Fl mode is used, the working range is extended (5 × 10–5–5 × 10–2 mol dm–3). The Fl methods were applied to the determination of NAC in pharmaceutical samples.

Determination of N-acetylcysteine in human plasma by gas chromatography—mass spectrometry

An automatic mass spectrometric method for the quantitation of N-acetylcysteine (NAC) in human plasma has been developed. NAC was extracted from plasma with ethyl acetate and derivatized in two steps with 2-praponol and pentafluoropropionic anhydride. The volatile derivative obtained was ideal for gas chromatographic—mass spectrometric analysis. Data obtained by analysing the plasma of healthy volunteers to whom 600 mg of NAC had been orally given are reported.

Analysis of thiols by HPLC after fluorescent prelabelling with 4-(6-methylnaphthalen-2-yl)-4-oxobuten-2-oic acid

The use of 4-(6-methylnaphthalen-2-yl)-4-oxobuten-2-oic acid as a fluorogenic reagent in pre-column derivatization for the high-performance liquid chromatography (HPLC) of biologically important thiols (L-cysteine, glutathione, N-acetylcysteine, homocysteine and mercaptopropionylglycine) was investigated. The aroylacrylic acid reacts selectively and rapidly (15 min. at room temperature) with the thiol compounds to give stable fluorescent adducts which can be separated by reversedphase HPLC and detected fluorometrically (λex 300nm); λem 445nm). The experimental conditions for the thiol derivatization and chromatographic separation are discussed. Applications to the determination of N-acetylcysteine, mercaptopropionylglycine and cysteine are described.

Determination of N-acetylcysteine, intact and oxidized, in plasma by column liquid chromatography and post-column derivatization

N-Acetylcysteine in plasma may exist as intact N-acetylcysteine (NAC) or be oxidized to disulphides, either as a dimer or mixed with other thiol-containing compounds. To prevent oxidation of NAC, whole blood was immediately centrifuged after collection and the plasma proteins were precipitated with perchloric acid. NAC was measured by direct injection of the supernatant into the chromatographic system and the oxidized forms, coupled to small sulphides (ONACS), were determined after reductive cleavage of all NAC disulphides in the supernatant with dithiothreitol before injection. The total plasma concentration of the compound, i.e., including the fraction coupled to proteins (ONACP), was assayed after an initial reduction of the disulphide linkages in plasma. After subsequent precipitation of proteins, the supernatant was directly injected. The chromatographic system was a reversed-phase column (C 18) with an acidic mobile phase. After a fast (<6 s) post-column reaction with pyrenemaleimide, NAC was detected by fluorimetry. The contribution to the band broadening by the reactor was about 10%. The limit of quantification of NAC in plasma was 240 n M, with an intra-assay precision of 14%.