scholarly journals Quantitative proton nuclear magnetic resonance method for simultaneous analysis of fluticasone propionate and azelastine hydrochloride in nasal spray formulation

2021 ◽  
Vol 8 (7) ◽  
pp. 210483
Author(s):  
Amal A. El-Masry ◽  
Dalia R. El-Wasseef ◽  
Manal Eid ◽  
Ihsan A. Shehata ◽  
Abdallah M. Zeid
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Fluticasone Propionate ◽  
Nasal Spray ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Proton Nuclear Magnetic Resonance ◽  
Nuclear Magnetic Resonance Method ◽  
Spray Formulation ◽  
Nuclear Magnetic

A facile, rapid, accurate and selective quantitative proton nuclear magnetic resonance ( 1 H-qNMR) method was developed for the simultaneous determination of fluticasone propionate (FLP) and azelastine hydrochloride (AZH) in pharmaceutical nasal spray for the first time. The 1 H-qNMR analysis of the studied analytes was performed using inositol as the internal standard and dimethyl sulfoxide- d 6 (DMSO- d 6 ) as the solvent. The quantitative selective proton signal of FLP was doublet of doublet at 6.290, 6.294, 6.316 and 6.319 ppm, while that of AZH was doublet at 8.292 and 8.310 ppm. The internal standard (inositol) produced a doublet signal at 3.70 and 3.71 ppm. The method was rectilinear over the concentration ranges of 0.25–20.0 and 0.2–15.0 mg ml −1 for FLP and AZH, respectively. No labelling or pretreatment steps were required for NMR analysis of the studied analytes. The proposed 1 H-qNMR method was validated efficiently according to the International Council on Harmonisation guidelines in terms of linearity, limit of detection, limit of quantification, accuracy, precision, specificity and stability. Moreover, the method was applied to assay the analytes in their combined nasal spray formulation. The results ensured the linearity ( r 2 > 0.999), precision (% RSD < 1.5), stability, specificity and selectivity of the developed method.

OBETICHOLIC ACID: AN INSIGHT INTO A QUANTITATIVE DETERMINATION AND METHODOLOGICAL VALIDATION THROUGH NUCLEAR MAGNETIC RESONANCE

2020 ◽  
pp. 179-190
Author(s):  
RAKESH SAHU ◽  
RAKHI MISHRA ◽  
CHANDANA MAJEE ◽  
AJAY KUMAR ◽  
RUPA MAZUMDER
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Quantitative Determination ◽  
Method Validation ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Proton Nuclear Magnetic Resonance ◽  
Obeticholic Acid ◽  
Relative Standard ◽  
Nuclear Magnetic

Objective: The research work unveils the use of nuclear magnetic resonance (NMR) technique for quantitative determination and method validation of obeticholic acid. As standard expository methodology for more up to date medications or formulations may not be available in pharmacopeias, hence it is fundamental need to create novel analytical procedures which should be precise and accurate. Methods: Proton (1H) and carbon (13C) NMR analysis were initially performed to confirm the preliminary authenticity of obeticholic acid API. Method validation was accomplished on the basis of standard guidelines for the parameters, in which tetramethylbenzene as an internal standard and deuterated dimethyl sulfoxide as a diluent were used to assess the obeticholic acid. Results: For the quantification of the drug, the proton nuclear magnetic resonance signals at 0.602 ppm and 6.86 ppm corresponding to the analyte proton of drug and internal standard respectively were used. The curve equation calculated from the regression method, the relative-standard-deviation and correlation-coefficient were found to be 0.743% and 0.9989 respectively, indicating good linearity. Consequently, the quantitative assay of the drug was found to be 99.91% in linearity with limit of detection and quantification values as 0.0773 mg and 0.2344 mg respectively, making successful the study of method validation for obeticholic acid. Conclusion: The advantage of the method was that no reference standard of analyte drug was required for quantification and method validation. The method is non-destructive and can be applied for quantification of drug in commercial pharmaceutical formulation products.

Determination of Ephedrine, Pseudoephedrine, and Norephedrine in Mixtures (Bulk and Dosage Forms) by Proton Nuclear Magnetic Resonance Spectroscopy

1995 ◽  
Vol 78 (4) ◽  
pp. 946-953 ◽  
Author(s):  
George M Hanna
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Dosage Forms ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
1H Nuclear Magnetic Resonance ◽  
Nuclear Magnetic

Abstract A simple, specific, and accurate 1H nuclear magnetic resonance (NMR) spectroscopic method has been developed for quantitative determination of the Ephedra alkaloids (−)-ephedrine, (+)-pseudoephedrine, and (±)-norephedrine, either singly or in mixtures with each other. Determination of individual alkaloids was carried out in D2O solution, with acetamide as internal standard. Although calculations were based on integrals for the C–CH3 protons, those for the N–CH3 and –CH–O– protons may also be useful, depending on the compound. Determination of diastereomeric cross-contamination of ephedrine and pseudoephedrine—or of the concentrations of these alkaloids in the presence or absence of (±)-norephedrine—was feasible by using the integrals for the –CH–O– protons after addition of a trace of DCI. Mean recoveries for ephedrine and pseudoephedrine from their respective synthetic mixtures with the internal standard (acet- amide) were ≥99.9 ± 0.6% (n = 10) and 99.6 ± 0.8% (n = 10) of the amount added. Recovery for pseudoephedrine from diastereomeric mixtures with ephedrine was &gt;99.4 ± 0.7% (n = 10) of the amount added, with as little as 1.92% still being measurable. Mean recovery of (±)-norephedrine from mixtures with ephedrine and pseudoephedrine was &gt;99.7 ± 2.5% (n = 4) of the amount added, with about 1% still being measurable. Application of the proposed NMR spectroscopic method to commercial dosage forms, including ephedrine sulfate injections and pseudoephedrine hydrochloride tablets, yielded assay results ranging from 97.8 to 100.2% (mean, 99.2%) and from 98.7 to 100.5% (mean, 99.7%) of declared, respectively.

scholarly journals Quantitative Analysis of Flavonoids in Glycyrrhiza uralensis Fisch by 1H-qNMR

2021 ◽  
Vol 2021 ◽  
pp. 1-6
Author(s):  
Ping Yu ◽  
Qian Li ◽  
Yanmei Feng ◽  
Yuying Chen ◽  
Sinan Ma ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Pulse Sequence ◽  
Quantitative Characteristic ◽  
Internal Standard ◽  
Proton Nuclear Magnetic Resonance ◽  
Experimental Result ◽  
Resonance Spectroscopy ◽  
Nuclear Magnetic

Objective. To establish a method for simultaneous determination of liquiritin, liquiritigenin, and isoliquiritinin glycyrrhizin using hydrogen nuclear magnetic resonance quantitative technology (1H-qNMR). Methodology. Deuterated dimethyl sulfoxide was used as the solvent, and dichloromethane was used as the internal standard. The probe temperature was 298.0 K, the pulse sequence was Zg30, the number of scans was 16, and relaxation delay (D1) was 10 s. Quantitative characteristic signal peaks were δ 4.891∼4.878 ppm, δ 8.187∼8.172 ppm, and δ 6.790∼6.776 ppm for liquiritin, isoliquiritin, and liquiritigenin, respectively. Results. The experimental result showed that the content of flavonoids in Licorice, from Chifeng, Inner Mongolia, was the highest. Conclusion. In this study, a new method for determination of three flavonoids in Licorice using 1H-qNMR was established. This experimental method has the advantages of accuracy, efficiency, and economy. It lays a foundation for the study on the determination of flavonoids content in licorice by proton nuclear magnetic resonance spectroscopy.

Stability-Indicating Proton Nuclear Magnetic Resonance Spectroscopic Assay Method for Furosemide in Tablets and Injections

1993 ◽  
Vol 76 (3) ◽  
pp. 526-530 ◽  
Author(s):  
George M Hanna ◽  
Cesar A Lau-Cam
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Degradation Product ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Butyl Alcohol ◽  
Proton Nuclear Magnetic Resonance ◽  
Assay Method ◽  
The Mean ◽  
Nuclear Magnetic

Abstract A simple, specific, and accurate proton nuclear magnetic resonance (1H-NMR) spectroscopic method has been developed for the identification and assay of furosemide and its degradation product, 4-chloro-5-sulfamoylanthranilic acid (CSA), in tablets and injections. Dissolution of the sample in D20-NaOD resulted in a solution yielding the required separation among the resonance signals of furosemide, CSA, and ferf-butyl alcohol, the internal standard. The mean ± SD recovery values of furosemide and CSA from 10 synthetic formulations were 99.6 ± 0.8 and 98.9 ± 1.7%, respectively. Commercial tablets (6 lots) and injections (5 lots) of furosemide were assayed by the proposed method and found to contain 53.1-99.8% furosemide and 0.3-45.2% CSA.

Stability-Indicating Proton Nuclear Magnetic Resonance Spectroscopic Method for Determination of S-Adenosyl-L-Methionine in Tablets

1995 ◽  
Vol 78 (2) ◽  
pp. 353-357 ◽  
Author(s):  
Larry K Revelle ◽  
D André d’Avignon ◽  
John C Reepmeyer ◽  
Richard C Zerfing
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Proton Nuclear Magnetic Resonance ◽  
Stability Indicating ◽  
Nmr Method ◽  
Relative Standard ◽  
The Stability ◽  
Nuclear Magnetic

Abstract We present a simple, accurate, stability-indicating nuclear magnetic resonance (NMR) method for determining active (S,S) and inactive (R,S) epimers of S-adenosyl-L-methionine (SAM) in tablets. The SCH3 resonances of SAM epimers were well resolved at 300 MHz. Individual assays of 5 SAM tablets gave SAM values of 101.3 ± 1.7% of declared amounts. Tablet solutions were assayed at a level of 8.0 mg/mL, but the method was linear for SAM concentrations ranging from 64 to 1 mg/mL (correlation coefficient, 0.9996). Reproducibility was indicated by a relative standard deviation of 0.33% for 6 replicate assays for total SAM at a concentration of 8 mg/mL. In contrast to the propietary liquid chromatographic (LC) method, which requires SAM as an external standard, the NMR method uses sodium trimethylsilylpropionate-d4 (TSP) both as an internal standard and as a chemical shift reference. The method was used to test the stability of SAM analytes under various pH levels and temperatures. We found 8% inactivation of SAM due to epimerization over a 24 h period at room temperature and pH 5. SAM solutions showed no detectable inactivation after 14 days when stored below 0°C.

Quantitative Nuclear Magnetic Resonance Spectroscopic Analysis of Two Commonly Used Gastrointestinal Tract Drugs

2020 ◽  
Vol 103 (5) ◽  
pp. 1208-1214
Author(s):  
Ramzia I Elbagary ◽  
Marwa A Fouad ◽  
Menna I Ezzeldin
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Quantitative Monitoring ◽  
Quantitative Nuclear Magnetic Resonance ◽  
Nuclear Magnetic

Background Two fast and precise quantitative nuclear magnetic resonance spectroscopic methods (qNMR) were established and evaluated for the determination of ondansetron (OND) and omeprazole (OMP) in bulk drugs and their pharmaceutical dosage forms. NMR spectra were established using dimethylsulfoxide (DMSO-d6) as a solvent and phloroglucinol as the internal standard. Proton NMR signals at 3.743, 3.811, and 5.670 ppm were used for quantitative monitoring purposes corresponding to OND, OMP, and phloroglucinol, respectively. In this study, the methods linearity, accuracy, limit of quantification, limit of detection, stability, and precision were validated as per International Conference on Harmonization (ICH) guidelines. Linearity ranges were 0.3–10 mg for OND and 1–10 mg for OMP. The student t-test and F-test were used for statistical evaluation. Herein, the proposed methods are useful and can be a successful practical appliance for OND and OMP determination in drug substances and their dosage forms.

scholarly journals Quantitative 1H Nuclear Magnetic Resonance Method for Assessing the Purity of Dipotassium Glycyrrhizinate

Molecules ◽  
2021 ◽  
Vol 26 (12) ◽  
pp. 3549
Author(s):  
Yuan-Yuan Zhang ◽  
Jie Zhang ◽  
Wen-Xuan Zhang ◽  
Yue Wang ◽  
Ying-Hong Wang ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Internal Standard ◽  
Resonance Method ◽  
Nuclear Magnetic Resonance Method ◽  
Limit Of Quantification ◽  
1H Nuclear Magnetic Resonance ◽  
Stability And Accuracy ◽  
Dipotassium Glycyrrhizinate ◽  
Nuclear Magnetic

A simple, rapid, accurate, and selective quantitative method based on 1H nuclear magnetic resonance (qNMR) was successfully established and developed for assessing the purity of dipotassium glycyrrhizinate (KG). In this study, using potassium hydrogen phthalate and fumaric acid as internal standard (IS), several important experimental parameters, such as relaxation delay and pulse angle, were explored. Reliability, specificity, linearity, limit of quantification, precision, stability, and accuracy were also validated. Calibration results obtained from qNMR were consistent with those obtained from HPLC coupled with ultraviolet detection. The proposed method, independent of the reference standard substance, is a useful, reliable, and practical protocol for the determination of KG and glycyrrhizin analogs.

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