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.

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.

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.

Determination of Insoluble, Soluble, and Total Dietary Fiber (CODEX Definition) by Enzymatic-Gravimetric Method and Liquid Chromatography: Collaborative Study

2012 ◽  
Vol 95 (3) ◽  
pp. 824-844 ◽  
Author(s):  
Barry V McCleary ◽  
Jonathan W DeVries ◽  
Jeanne I Rader ◽  
Gerald Cohen ◽  
Leon Prosky ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Water Soluble ◽  
Official Method ◽  
Soluble Dietary Fiber ◽  
Total Dietary Fiber ◽  
Food Ingredients ◽  
Aoac Official

Abstract A method for the determination of insoluble (IDF), soluble (SDF), and total dietary fiber (TDF), as defined by the CODEX Alimentarius, was validated in foods. Based upon the principles of AOAC Official MethodsSM 985.29, 991.43, 2001.03, and 2002.02, the method quantitates water-insoluble and water-soluble dietary fiber. This method extends the capabilities of the previously adopted AOAC Official Method 2009.01, Total Dietary Fiber in Foods, Enzymatic–Gravimetric– Liquid Chromatographic Method, applicable to plant material, foods, and food ingredients consistent with CODEX Definition 2009, including naturally occurring, isolated, modified, and synthetic polymers meeting that definition. The method was evaluated through an AOAC/AACC collaborative study. Twenty-two laboratories participated, with 19 laboratories returning valid assay data for 16 test portions (eight blind duplicates) consisting of samples with a range of traditional dietary fiber, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 10.45 to 29.90%. Digestion of samples under the conditions of AOAC 2002.02 followed by the isolation, fractionation, and gravimetric procedures of AOAC 985.29 (and its extensions 991.42 and 993.19) and 991.43 results in quantitation of IDF and soluble dietary fiber that precipitates (SDFP). The filtrate from the quantitation of water–alcohol-insoluble dietary fiber is concentrated, deionized, concentrated again, and analyzed by LC to determine the SDF that remains soluble (SDFS), i.e., all dietary fiber polymers of degree of polymerization = 3 and higher, consisting primarily, but not exclusively, of oligosaccharides. SDF is calculated as the sum of SDFP and SDFS. TDF is calculated as the sum of IDF and SDF. The within-laboratory variability, repeatability SD (sr), for IDF ranged from 0.13 to 0.71, and the between-laboratory variability, reproducibility SD (sR), for IDF ranged from 0.42 to 2.24. The within-laboratory variability sr for SDF ranged from 0.28 to 1.03, and the between-laboratory variability sR for SDF ranged from 0.85 to 1.66. The within-laboratory variability sr for TDF ranged from 0.47 to 1.41, and the between-laboratory variability sR for TDF ranged from 0.95 to 3.14. This is comparable to other official and approved dietary fiber methods, and 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.

Collaborative Study of the Quantitative Gas-Liquid Chromatographic Determination of Fusel Oil and Other Components in Whisky

1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger
Keyword(s):  
Ethyl Acetate ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Official Method ◽  
Fusel Oil ◽  
Fusel Alcohols ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.

scholarly journals Comparison of Babcock and Ether Extraction Methods for Determination of Fat Content of Cream: Collaborative Study

1996 ◽  
Vol 79 (4) ◽  
pp. 907-916 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Extraction Method ◽  
Collaborative Study ◽  
Extraction Methods ◽  
Fat Content ◽  
Official Method ◽  
Ether Extraction ◽  
Aoac Official ◽  
The Difference ◽  
Aoac Official Method

Abstract A modified Mojonnier ether extraction method for determination of the fat content of cream was developed based on the method for milk (AOAC Official Method 989.05). The cream Babcock method (AOAC Official Method 920.111 B-C) was modified to harmonize with the milk Babcock method (AOAC Official Method 989.04) and to clarify procedural details. Using the AOAC collaborative study format, 10 laboratories tested 9 pairs of blind duplicate heat-treated cream samples with a fat range of 30-45% using both methods. The statistical performance (invalid and outlier data removed) was as follows: mean % fat = 37.932, sr = 0.125, sR = 0.151, RSDr = 0.330, RSDR = 0.398, r = 0.354, and R = 0.427 for the ether extraction method. For the Babcock method, mean % fat = 38.209, sr = 0.209, SR = 0.272, RSDr = 0.548, RSDR = 0.712, r = 0.592, and R = 0.769. Average test results for fat from the Babcock method were 0.277% (absolute fat) greater than for the Mojonnier ether extraction method. The difference between methods, as a percentage of the average fat content of the samples, was 0.73%. This agrees with differences observed between the 2 methods for milk when 10 to 17 laboratories tested 7 milk samples in blind duplicate at bimonthly intervals over a 4-year period (average difference 0.029% fat, 0.78% as a percentage of average fat content). The Mojonnier ether extraction and Babcock methods for fat in cream have been adopted by AOAC INTERNATIONAL. The new Babcock method replaced the AOAC Official Method 920.111 B-C.

Determination of Maleic Hydrazide Residues in Tobacco and Vegetables

1973 ◽  
Vol 56 (5) ◽  
pp. 1164-1172
Author(s):  
Milan Ihnat ◽  
Robert J Westerby ◽  
Israel Hoffman
Keyword(s):  
Standard Deviation ◽  
Present Method ◽  
Maleic Hydrazide ◽  
Collaborative Study ◽  
Official Method ◽  
Sample Weight ◽  
Relative Standard ◽  
The Mean ◽  
Pipe Tobacco

Abstract The distillation-spectrophotometric method of Hoffman for determining maleic hydrazide has been modified to include a double distillation and was applied to the determination of 1–30 ppm maleic hydrazide residues in tobacco and vegetables. Recoveries of 1–23 μg added maleic hydrazide were independent of weight of maleic hydrazide, but did depend on sample and sample weight. The following recoveries were obtained from 0.5 g sample: pipe tobacco, 84%; commercially dehydrated potato, 83%; cigar tobacco, 81%; dried potato, 76%; fluecured tobacco, 73%; dried carrot, 71%. In the absence of sample, the recovery was 82%. When appropriate standard curves were used, maleic hydrazide levels determined in tobacco samples were essentially independent of sample weight in the range 0.1–3 g. The mean relative standard deviation for a variety of field-treated and fortified tobacco samples containing 1–28 ppm maleic hydrazide was 3%. The precision and sensitivity of this procedure seem to be substantial improvements over official method 29.111–29.117. It is recommended that the present method be subjected to a collaborative study.

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.

Collaborative Study of the Determination of Phosphorus in Gelatin, Dessert Preparations, and Mixes

1972 ◽  
Vol 55 (3) ◽  
pp. 581-582
Author(s):  
Roger G Burkepile
Keyword(s):  
Collaborative Study ◽  
Official Method ◽  
Standard Samples ◽  
Preliminary Work ◽  
Aoac Method ◽  
Standard Deviations

Abstract A collaborative study of the proposed method for phosphorus in gelatin, dessert preparations, and mixes has been conducted. The present AOAC method for phosphorus in fertilizers, 2.023–2.025(a), was modified for this study. Preliminary work by the Associate Referee involving 4 phosphorus standard samples compared the proposed method with the official final action AOAC method for gelatin, 23.004. Additionally, phosphorus standard spikes in gelatin at the 1 and 10 mg P2O5, levels were determined by the proposed method. The proposed method is faster and more sensitive than the official method and is as accurate. Five collaborators and the Associate Referee analyzed 4 prepared samples containing various levels of phosphorus by the proposed method. The standard deviations varied from 0.005 for a 225 Bloom gelatin containing an average of 0.273% P2O5 to 0.016 for a strawberry-flavored commercial gelatin with added lecithin containing an average of 0.110% P2O5. The proposed method has been adopted as official first action to replace 23.004, which was repealed, 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.

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