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.

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.

Atomic Absorption Spectrophotometric Method for Determination of Water-Soluble Copper in Water-Insoluble Copper Fungicides: CIPAC Collaborative Study. Comparison with Bathocuproine Method

1981 ◽  
Vol 64 (1) ◽  
pp. 75-78
Author(s):  
F Sánchez Rasero ◽  
◽  
P G Balayannis ◽  
H P Beyers ◽  
E Celma ◽  
...  
Keyword(s):  
Atomic Absorption ◽  
Collaborative Study ◽  
The United States ◽  
Atomic Absorption Spectrophotometry ◽  
Water Soluble ◽  
Absorption Spectrophotometry ◽  
Aas Method ◽  
Standard Deviations ◽  
The Difference

Abstract An atomic absorption spectrophotometric (AAS) method was collaboratively studied by 8 laboratories from Africa, the United States, Australia, and Europe. The samples were dispersed in deionized water. After centrifuging and filtering, the water-soluble copper in the filtrate was acidified and measured by atomic absorption spectrophotometry, in an airacetylene flame, at 324.7 nm. The results from 7 laboratories were satisfactory and no unfavorable comments were received. Repeatability standard deviations ranged from 0.005 to 0.023, and reproducibility standard deviations ranged from 0.012 to 0.062. When compared with the bathocuproine method, the difference in bias between both methods is not significant. They were both adopted as full CIPAC methods, with the bathocuproine method as the referee method. Both methods have been adopted official first action.

Gas-Liquid Chromatographic Quantitation of Pheneyclidine.HCl in Powders: Collaborative Study

1979 ◽  
Vol 62 (3) ◽  
pp. 560-563
Author(s):  
Charles C Clark
Keyword(s):  
Aqueous Solution ◽  
Collaborative Study ◽  
Internal Standard ◽  
Water Soluble ◽  
Standard Deviations ◽  
Hcl Concentration ◽  
Liquid Chromatographic

Abstract Six laboratories collaboratively studied a method for the quantitative gas-liquid chromatographic (GLC) determination of pheneyclidine. HCl in powders. The pheneyclidine.HCl and other water-soluble compounds are dissolved in dilute HC1. A portion of the aqueous solution is made weakly basic with K2HPO4, and the organic-soluble compounds are extracted in CHCI3 for the GLC determination of the pheneyclidine.HCl. Eicosane (n-C20) is incorporated in the extracting CHC13 as an internal standard. The samples collaboratively studied included samples of known pheneyclidine. HCl concentration and one sample of unknown purity. Recoveries ranged from 92.1 to 104% and per cent standard deviations from 1.05 to 3.39. The method was adopted as official first action.

Collaborative Study of the Spectrophotometric Determination of Procainamide Hydrochloride

1976 ◽  
Vol 59 (4) ◽  
pp. 807-810
Author(s):  
Jeffrey C Hamm
Keyword(s):  
Sodium Hydroxide ◽  
Acid Medium ◽  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Dosage Forms ◽  
Standard Deviations

Abstract The USP analysis for procainamide HCl is titrimetric and relatively nonspecific, capsule and tablet dyes may interfere, and the method is not applicable to coated tablets. In the spectrophotofluorometric method the sample deteriorates when exposed to a xenon source. In the ultraviolet spectrophotometric method reported here, the sample is dispersed in acid medium, possible interferences are extracted in chloroform, base is added, procainamide is extracted in chloroform, the residue is dissolved in sodium hydroxide, and the compound is measured by absorption at 272 nm and comparison with a standard. Recoveries of standards added to capsule, tablet, and injection composites ranged from 99.3 to 102%. Twelve collaborators reported duplicate assay results for all 3 dosage forms with per cent standard deviations for 5 samples ranging from 1.01 to 1.27%. The method has been adopted as official first action.

Quantitative Ultraviolet Determination of Amiben in Dry Granular and Liquid Formulations: Collaborative Study

1970 ◽  
Vol 53 (6) ◽  
pp. 1155-1159
Author(s):  
Joax W Brunstad
Keyword(s):  
Sodium Salt ◽  
Collaborative Study ◽  
Standard Deviations

Abstract Amiben is determined as the sodium salt in 1% NaOH at 297 nm. Prepared materials and technical formulations containing 0-60 μg amiben/ml were analyzed in a collaborative study. Standard deviations for technical samples ranged from 0.05 to 0.45 and for prepared samples from 0.02 to 0.35. The method is recommended for adoption as official first action.

scholarly journals Utilization of Kalpataru Flower Extract (Hura crepitans Linn) as an Alternative Acid Base Indicator

2020 ◽  
Vol 9 (3) ◽  
pp. 148-157
Author(s):  
Bayu Riswanto ◽  
Sitti Aminah
Keyword(s):  
Strong Acid ◽  
Weak Acids ◽  
Acid Base ◽  
Flower Extract ◽  
Weak Bases ◽  
Base Solution ◽  
Acid Base Titration ◽  
Hura Crepitans ◽  
Dark Green ◽  
Strong Acids

Kalpataru flower (Hura crepitans Linn) is an anthocyanin-containing plant. This study aims to utilize extract from the kalpataru flower as an alternative acid base indicator and determine the type of acid-base titration suitable for extracting the kalpataru flower indicator. Kalpataru flowers are macerated with methanol solvent for around 2 hours. Kalpataru flower extract was tested as an indicator in acid-base solution, buffer, and compared with phenolphthalein and methyl orange for acid-base titration, namely: strong acids with strong bases, weak acids with strong bases, and weak bases with strong acids. The results obtained in this study were: indicator extract of brownish yellow kalpataru flowers, in strong red acids, in strong bases of dark green, in weak pink acids, and in weak bases in light green. In the buffer, the indicator extract of the kalpataru flower has a range of pH pH 4-5 (pink-colorless) and pH 9-11 (yellowish green-dark green). The indicator of kalpataru flower extract can be used on strong acid titration with strong bases, weak acids with strong bases and weak bases with strong acids. Kalpataru flower extract can be used as an acid-base indicator.

Colorimetric Determination of the Progestational Steroids in Contraceptive Tablets

1970 ◽  
Vol 53 (4) ◽  
pp. 831-833
Author(s):  
John Y P Wu
Keyword(s):  
Oral Contraceptive ◽  
Medroxyprogesterone Acetate ◽  
Collaborative Study ◽  
Chloroform Extract ◽  
Colorimetric Determination ◽  
Standard Deviations ◽  
Isonicotinyl Hydrazide ◽  
Norethindrone Acetate

Abstract Norethindrone, norethindrone acetate, dimethisterone, medroxyprogesterone acetate, and norethynodrel are determined in oral contraceptive tablets. For the first 4 compounds, a chloroform extract of the tablets is treated directly with isonicotinyl hydrazide reagent to produce a stable color which is measured at 380 nm. The chloroform extract of norethynodrel tablets is isomerized before the reagent is added. An intralaboratory study gave good results, with standard deviations of 0.74 to 1.21%. A collaborative study is recommended.

Collaborative Study of the Gas-Liquid Chromatographic Method for Determination of Stereochemical Composition of Amphetamine

1972 ◽  
Vol 55 (1) ◽  
pp. 146-148
Author(s):  
Clyde E Wells
Keyword(s):  
Column Chromatography ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Good Precision ◽  
Liquid Chromatographic Method ◽  
Precision And Accuracy ◽  
Standard Deviations ◽  
Liquid Chromatographic ◽  
Amphetamine Sulfate

Abstract Eight laboratories collaboratively studied a method for the quantitative GLC determination of d- and l-amphetamine in tablets. The drugs are separated from tablet excipients by column chromatography and reacted with Ntrifluoroacetyl-( 0-prolyl chloride, and the resulting derivatives are analyzed by GLC. The samples consisted of commercial d-amphetamine sulfate tablets (with and without butabarbital), dl-amphetamine sulfate tablets, and a mixed d- and l-amphetamine sulfate standard. Recoveries were acceptable, and the standard deviations never exceeded 0.64%. The results demonstrate that the method gives good precision and accuracy, and the method is recommended for adoption as official first action.

Collaborative Study of a Gas-Liquid Chromatographic Method for the Determination of Water-Soluble Menadione (Vitamin K3) in Feed Premixes

1973 ◽  
Vol 56 (5) ◽  
pp. 1277-1280
Author(s):  
Victor W Winkler
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Water Soluble ◽  
Vitamin K3 ◽  
Menadione Sodium Bisulfite ◽  
Liquid Chromatographic Method ◽  
Coefficients Of Variations ◽  
Liquid Chromatographic ◽  
Pyrolytic Product

Abstract A GLC method for the determination of menadione bisulfite addition products in feed premixes was tested by 8 laboratories. Menadione sodium bisulfite complex (trihydrate) is extracted with methanol containing 1 mg diethyl phthalate/ml as internal standard and injected directly onto a 2% OV-17 (silylated) GLC column. The principle of the method is on-column pyrolysis of menadione bisulfite and subsequent GLC analysis of the pyrolytic product, menadione. The method is simple, rapid, and free from interference. The average recovery values for 4 samples at 16.0, 14.4, 4.0, and 3.6 g/lb ranged from 95.8 to 100.4% with coefficients of variations between 5.5 and 6.5%. The method has been adopted as interim official first action.

Sign in / Sign up

Export Citation Format

Share Document