Proton Magnetic Resonance Spectroscopic Method for Determination of Phenylbutazone and Oxyphenbutazone in Tablets

1988 ◽  
Vol 71 (3) ◽  
pp. 525-527
Author(s):  
Sajid Husain ◽  
M Kifayatullah ◽  
R NAGESWARA RAO
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Proton Magnetic Resonance ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Aromatic Proton ◽  
British Pharmacopoeia ◽  
Standard Deviations ◽  
Proton Resonances

Abstract A simple, specific, and rapid 'H nuclear magnetic resonance spectroscopic method for the assay of phenylbutazone and oxyphenbutazone is described. Spectra are recorded in CDC13 containing 1,3- dichloro-5-nitrobenzene as an internal standard. The aromatic proton resonances for the standard, at 57.7 and 8.2, are well separated from those of phenylbutazone and oxyphenbutazone, which are in the region of 56.5-7.3 ppm. Average percent recoveries of phenylbutazone and oxyphenbutazone were 98.9 and 98.6 with standard deviations of 0.6 and 0.7, respectively. Commercial formulations were analyzed and the results obtained by the proposed method closely agreed with those found by the British Pharmacopoeia method

Proton Magnetic Resonance Spectroscopic Determination of Disulfiram: Collaborative Study

1978 ◽  
Vol 61 (1) ◽  
pp. 55-59
Author(s):  
Eric B Sheinin ◽  
Walter R Benson
Keyword(s):  
Magnetic Resonance ◽  
Proton Magnetic Resonance ◽  
Drug Product ◽  
Spectroscopic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Spectroscopic Determination ◽  
Standard Deviations ◽  
Bulk Drug

Abstract A proton magnetic resonance spectroscopic method for determining disulfiram in the bulk drug product and in the formulated material was collaboratively studied. The method depends on the use of chloroform-d as a solvent and hexamethylcyclotrisiloxane as the internal standard. No interference from tablet excipients was observed. The method is rapid and specific. Eighteen laboratories analyzed duplicate samples of a bulk drug product, a 250 mg tablet composite, and a 500 mg tablet composite. The average per cent results and standard deviations were 99.7±1.4, 100.9±2.0, and 99.9±2.2, respectively.

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 >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 >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.

Application of ^-Nuclear Magnetic Resonance Spectroscopic Method for Quinidine to Simultaneous Determination of Quinidine and Dihydroquinidine in Quinidine Sulfate Tablets

1988 ◽  
Vol 71 (6) ◽  
pp. 1118-1121
Author(s):  
George M Hanna ◽  
Cesar A Lau-Cam
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Deuterated Chloroform ◽  
Structural Differences ◽  
Commercial Source ◽  
Quinidine Sulfate ◽  
Nuclear Magnetic

Abstract Based on the structural differences between quinidine and dihydroquinidine, a 'H-nuclear magnetic resonance spectroscopic method previously reported for quinidine drug substance was modified and shown to be applicable to the quantitative determination of both compounds in quinidine sulfate tablets. Deuterated chloroform was used as the solvent and hexamethylcyclotrisiloxane served as an internal standard. The average recovery and standard deviation of quinidine sulfate (calculated as the sum of quinidine sulfate plus dihydroquinidine sulfate) from synthetic formulations was 98.94 ± 0.43% (n = 10). Five lots of 200 mg tablets of quinidine sulfate from one commercial source were found to contain from 92.9 to 95.8% quinidine sulfate, and from 1.1 to 7.0% dihydroquinidine sulfate

Nuclear Magnetic Resonance Spectroscopic Determination of Dicyclomine Hydrochloride in Tablet, Capsule, and Injection Dosage Forms

1984 ◽  
Vol 67 (2) ◽  
pp. 222-224 ◽  
Author(s):  
George M Hanna
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Chloral Hydrate ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Dosage Forms ◽  
Spectral Determination ◽  
Extraction Step ◽  
Nuclear Magnetic

Abstract A rapid and specific nuclear magnetic resonance (NMR) spectroscopic method was developed for determining dicyclomine hydrochloride in tablet, capsule, and injection dosage forms. The method consists of an extraction step with chloroform, evaporation of the solvent, addition of maleic acid as an internal standard, dissolution of the mixture in deuterated chloroform-deuterated acetone (40 + 60), NMR spectral determination, and integration of the peaks of interest. The concentration of dicyclomine hydrochloride in the dosage form was calculated from the integral values for the peaks of the test compound and the internal standard. The average recovery value ±the standard deviation (n = 5) of dicyclomine hydrochloride added to synthetic samples was 99.7 ± 0.9% (coefficient of variation 0.9%). The assay values for various commercial tablets, capsules, and injectables analyzed by using the proposed method differed in all cases by <1% from those obtained by using the USP XX titrimetric method. There was no interference from stearate, an excipient found in tablets and capsules, or from chloral hydrate, a preservative found in injectables.

Nuclear Magnetic Resonance Spectroscopic Method for Determination of Penicillamine in Capsules

1981 ◽  
Vol 64 (5) ◽  
pp. 1174-1178
Author(s):  
James Nelson
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Spectroscopic Method ◽  
Internal Standard ◽  
Sodium Saccharin ◽  
Phenyl Proton ◽  
Nuclear Magnetic

Abstract A rapid and specific nuclear magnetic resonance (NMR) spectroscopic method for the determination of penicillamine in capsules is presented. The sample is directly dissolved in D2O and its spectrum recorded on a 90 MHz instrument. The 2 singlets appearing at 1.58–1.64 ppm, due to the nonequivalent gem-dimethyl groups, were integrated and compared with the integral obtained for the phenyl proton signals of sodium saccharin, which is the internal standard. The results obtained by the proposed method closely agreed with those found by the method of USP XX.

Nuclear Magnetic Resonance Spectroscopic Determination of Methoxyflurane

1981 ◽  
Vol 64 (5) ◽  
pp. 1154-1157
Author(s):  
Kermit W Henry
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Carbon Tetrachloride ◽  
Magnetic Resonance ◽  
Dimethyl Sulfoxide ◽  
Spectroscopic Method ◽  
Proton Nmr ◽  
Internal Standard ◽  
Nmr Spectrum ◽  
Nuclear Magnetic

Abstract A simple, rapid nuclear magnetic resonance (NMR) spectroscopic method for quantitatively determining methoxyflurane was developed. The proton NMR spectrum of methoxyflurane in carbon tetrachloride exhibited a well defined triplet at 5.67 ppm and a sharp singlet at 3.68 ppm. Using dimethyl sulfoxide (DMSO) as an internal standard, methoxyflurane was quantitated by comparing the integral for the singlet of methoxyflurane with the integral for the singlet of DMSO at 2.60 ppm. The method was accurate to concentrations as low as 1‑2%, and results agreed with those obtained by the NF XIV method

Nuclear Magnetic Resonance Analysis of Pharmaceuticals. IX. Methenamine and Methenamine Mandelate in Tablets

1973 ◽  
Vol 56 (3) ◽  
pp. 669-673
Author(s):  
John W Turczan ◽  
Bruce A Goldwitz
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Maleic Acid ◽  
Mandelic Acid ◽  
Internal Standard ◽  
Solvent System ◽  
Nuclear Magnetic Resonance Analysis ◽  
Resonance Analysis ◽  
Nuclear Magnetic

Abstract An NMR procedure is described by which methenamine and mandelic acid are simultaneously determined in methenamine and methenamine mandelate tablets. Maleic acid was chosen as the internal standard and dimethylformamide-acetone-acetonitrile (10+25+65) as the solvent. The solvent system was selected to resolve the problems of solubility of methenamine and its salt with mandelic acid, overlapping of the resonance signals of the components, and potential decomposition of methenamine. Known standard and commercial preparations were analyzed and the results were compared to those of official USP and NF procedures. The NMR technique, when applied to the determination of methenamine and methenamine mandelate in tablets, is rapid, simple, and specific and can provide an assay with an accuracy of 1–2%.

Simultaneous Determination of Ibuprofen and Acetaminophen in Pharmaceutical Preparations by Proton Magnetic Resonance Spectroscopy

1994 ◽  
Vol 77 (6) ◽  
pp. 1443-1446
Author(s):  
Sajid Husain ◽  
M Kifayatullah ◽  
R Sekhar
Keyword(s):  
Magnetic Resonance ◽  
Magnetic Resonance Spectroscopy ◽  
Simultaneous Determination ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Aromatic Proton ◽  
Butyl Alcohol ◽  
Resonance Spectroscopy ◽  
Specific Method

Abstract A simple, rapid, and specific method for simultaneous determination of ibuprofen and acetaminophen in pharmaceutical preparations by 1H Fourier transform nuclear magnetic resonance spectroscopy was developed using methyl and aromatic proton signal areas against ferf-butyl alcohol as internal standard. Average recoveries of ibuprofen and acetaminophen were 99.2 and 98.6%, with standard deviations of ± 0.76 and ± 0.81, respectively. The results were compared with those obtained using the procedure recommended by the British Pharmacopoeia and were in close agreement.

Quantitative Determination of Chlorpromazine. HC1 in Tablets, Spansules, Injectables, and Bulk Chemical by Nuclear Magnetic Resonance Spectroscopy

1978 ◽  
Vol 61 (1) ◽  
pp. 52-54
Author(s):  
John E Zarembo ◽  
Richard J Warren ◽  
David B Staiger
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Internal Standard ◽  
Resonance Spectroscopy ◽  
Internal Standards ◽  
Tetramethylammonium Bromide ◽  
Bulk Chemical ◽  
Characteristic Signal ◽  
Nuclear Magnetic

Abstract A nuclear magnetic resonance (NMR) procedure is described for the quantitative analysis of chlorpromazine. HC1 in bulk chemical as well as in final dosage forms—tablets, spansules, and injectables. The method is based on measurement of a characteristic signal of chlorpromazine relative to an internal standard. Three different internal standards are specified: Cyclohexane was selected because of the convenience and rapidity with which samples could be prepared for assay. Piperonal was used to verify the method and to show that precision and accuracy were not affected by the volatility of the cyclohexane. Tetramethylammonium bromide was used as an internal standard for Thorazine injectable. No interferences were found from stearates and other tablet excipients. The NMR procedure provides a simple, direct, and specific assay with a precision of ± 1–2%.

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