On-Column Periodate Reaction Method for Analysis of Ephedrine Sulfate in Solid Dosage Forms: Collaborative Study

1980 ◽  
Vol 63 (4) ◽  
pp. 692-695
Author(s):  
Charles C Clark ◽  
◽  
W Brittan ◽  
C Hezeau ◽  
D Hughes ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Dosage Forms ◽  
Water Soluble ◽  
Solid Dosage Forms ◽  
Commercial Sample ◽  
Reaction Method ◽  
Solid Dosage ◽  
Weak Bases ◽  
Strong Acids

Abstract Seven laboratories collaboratively studied a method for the quantitative ultraviolet (UV) determination of ephedrine sulfate in solid dosage forms. Ephedrine is separated from water-soluble impurities and strong acids by elution from a weakly basic Celite column, and further cleaned up by retention on a weakly acidic column while the weak acids, weak bases, and organic-soluble neutrals are eluted. Ephedrine is eluted from the column after neutralization with NH3 and is converted to benzaldehyde via an on-column periodate reaction. The samples collaboratively studied consisted of 3 synthetic preparations of known ephedrine sulfate concentrations and 2 commercial preparations containing ephedrine sulfate. One commercial sample was submitted as a blind duplicate. Recoveries for the synthetic preparations averaged 101.7, 101.2, and 100.5% for mixtures containing 7.93, 9.35, and 6.85% ephedrine sulfate, respectively. The means and standard deviations for the commercial preparations were 24.72 ± 0.376 mg/dosage unit for the preparation labeled to contain 25 mg/dosage unit, and 22.46 ± 0.643 and 22.29 ± 0.339 mg/dosage unit for the blind duplicate labeled to contain 24 mg/dosage unit. The method has been adopted as official first action.

Collaborative Study of an On-Column Periodate Reaction Method for the Analysis of Phenylpropanolamine Hydrochloride in Elixirs

1973 ◽  
Vol 56 (1) ◽  
pp. 100-104
Author(s):  
Charles C Clark
Keyword(s):  
Collaborative Study ◽  
Water Soluble ◽  
Weak Acids ◽  
Reaction Method ◽  
Weak Bases ◽  
Phenylpropanolamine Hydrochloride ◽  
Standard Deviations ◽  
Strong Acids

Abstract Twelve laboratories collaboratively studied a method for the quantitative UV determination of phenylpropanolamine HC1 in elixirs. The phenylpropanolamine is separated from water-soluble impurities and strong acids by elution from a weakly basic Celite column. Further cleanup is accomplished by retention of the phenylpropanolamine on a weakly acidic column while the weak acids, weak bases, and organic-soluble neutrals are eluted. Phenylpropanolamine is eluted from the column after neutralization with NH3 and is converted to benzaldehyde via an on-column periodate reaction. The samples collaboratively studied consisted of 2 commercial and 2 synthetic elixirs. Recoveries of the synthetic elixirs averaged 100.1 and 101.8% for mixtures containing 5.05 and 12.52 mg/5 ml phenylpropanolamine HC1, respectively. The means and standard deviations for the commercial preparations were 4.75 ±0.12 and 12.34±0.16 mg/5 ml. The method has been adopted as official first action.

Collaborative Study of an On-Column Periodate Reaction Method for the Determination of Ephedrine Sulfate in Sirups

1975 ◽  
Vol 58 (4) ◽  
pp. 852-855
Author(s):  
Charles C Clark
Keyword(s):  
Collaborative Study ◽  
Water Soluble ◽  
Official Method ◽  
Weak Acids ◽  
Reaction Method ◽  
Weak Bases ◽  
Neutral Compounds ◽  
Phenylpropanolamine Hydrochloride ◽  
Strong Acids

Abstract Fifteen laboratories collaboratively studied a method for the quantitative ultraviolet determination of ephedrine sulfate in sirups. Ephedrine is separated from water-soluble impurities and strong acids by elution from a weakly basic Celite column. Further cleanup is accomplished by retention of the ephedrine on a weakly acidic column while the weak acids, weak bases, and organic-soluble neutral compounds are eluted. Ephedrine is eluted from the column after neutralization with NH3 and is converted to benzaldehyde via an on-column periodate reaction. The samples collaboratively studied consisted of 2 commercial ephedrine-containing sirups and 2 commercial non-ephedrine-containing sirups to which ephedrine was added. Recoveries for the spiked sirups averaged 100.7 and 100.3% for mixtures containing 2.5 and 5.0 mg ephedrine sulfate/ml, respectively. The means and standard deviations for the commercial preparations were 4.088 ± 0.068 and 2.375 ± 0.053 mg/ml. The method has been adopted as official first action and has been incorporated into the official method for phenylpropanolamine hydrochloride, 38.199–38.203.

Determination of Aspirin and Salicylic Acid by Reverse-Phase Liquid Chromatography

1987 ◽  
Vol 70 (6) ◽  
pp. 964-966
Author(s):  
Dorothy R Heidemann ◽  
Edward S Schulenberg ◽  
William H Smith
Keyword(s):  
Salicylic Acid ◽  
Dosage Forms ◽  
Solid Dosage Forms ◽  
Reverse Phase ◽  
Solid Dosage ◽  
Reverse Phase Liquid Chromatography ◽  
Sample Extraction ◽  
Phase Liquid ◽  
Phase Column

Abstract Buffered solid dosage forms containing aspirin, magnesium hydroxide, and aluminum hydroxide are blended with acidic ethanol to extract the aspirin and salicylic acid rapidly. The resulting preparation is then immediately injected onto a 4.6 mm x 3 cm 5 (im reverse-phase column. Aspirin and free salicylic acid are determined simultaneously. The run time is <2 min. The total time from the initiation of sample extraction to completion of the separation is <5 min.

Gas Chromatographic Separation and Quantitative Estimation of Barbiturate Mixtures in Solid Dosage Forms

1968 ◽  
Vol 51 (3) ◽  
pp. 619-621
Author(s):  
John L Allen
Keyword(s):  
Chromatographic Separation ◽  
Chromatographic Method ◽  
Quantitative Estimation ◽  
Collaborative Study ◽  
Internal Standard ◽  
Dosage Forms ◽  
Solid Dosage Forms ◽  
Solid Dosage ◽  
Gas Chromatographic Method ◽  
Gas Chromatographic Separation

Abstract A gas chromatographic method has been described for the analysis of mixed barbiturates in solid dosage forms. Analysis on a 10% SE-30 column gave good separations for butabarbital, amobarbital, secobarbital, pentobarbital, and/or phenobarbital; amobarbital is not separated adequately from pentobarbital. An internal standard, mephobarbital, is used to minimize injection errors. The method gives both good quantitative and qualitative results on the barbiturates investigated. Two synthetic tablet mixtures were analyzed by this procedure and recoveries were 98—103%. It is recommended that the method be subjected to collaborative study.

Novel First Order Derivative UV Spectrophotometric Method for the Determination of Glimepiride in Solid Dosage Forms

2018 ◽  
Vol 8 (3) ◽  
Author(s):  
Santosh Karajgi . ◽  
Sunayana Mali ◽  
Ramaling Kotnal
Keyword(s):  
Dosage Forms ◽  
Order Derivative ◽  
Simultaneous Estimation ◽  
Drug Form ◽  
Solid Dosage Forms ◽  
First Order ◽  
Solid Dosage ◽  
Tablet Dosage ◽  
Guide Lines

Objective: An easy, perfect, specific and exact process has been studied for the simultaneous estimation of Glimepiride pure drug form as well as tablet dosage forms. Methods: A UV method for quantitative evaluation of Glimepiride by first order derivative peak detect method for determination in bulk as well as tablet dosage form is reported as there was a need to expand novel methods to analyze the drug. Results: Glimepiride has absorbance first derivative maxima at 225 nm in Methanol. Glimepiride follows Beer’s law in concentration range of 5-25µg/ml. The outcomes of the study were validated statistically and recovery studies were performed as per ICH guide lines. Conclusion: Thus the projected method can be applied competently for the estimation of Glimepiride in regular analysis in its dosage forms.

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