Organic Acids in Vanilla Extract

1963 ◽  
Vol 46 (4) ◽  
pp. 626-633 ◽  
Author(s):  
J Fitelson

Abstract I. Paper Chromatographic Method Five samples of vanilla extract were submitted for collaborative study. Collaborators reported that the paper chromatographic method was simple and gave considerable information. Comparison with the results obtained by two-dimensional paper chromatography on the same five samples showed good agreement; the organic acid method disclosed adulteration more definitely in some samples. The method was recommended for adoption as official, first action. II. Gradient Elution Method In the Gradient Elution Method, the organic acids are separated from the extract by an ion exchange resin and eluted with increasing concentrations of formic acid. Vanilla extract shows a typical elution pattern with 4 peaks. Results are reported on 87 authentics (54 previously published, 33 new samples). Collaborative study on 4 samples resulted in several modifications. The method was recommended as official, first action as a check method for adulterated samples.

1964 ◽  
Vol 47 (3) ◽  
pp. 558-560 ◽  
Author(s):  
J Fitelson

Abstract Further collaborative studies were made of the gradient elution and paper chromatographic methods for organic acids in vanilla extract, both adopted as official, first action in 1962. The gradient elution method was studied by six collaborators on three samples. All six detected the presence of added foreign acid. The paper chromatographic method was studied by 16 collaborators on four unknown samples and one reference standard vanilla. Results were very good. It is recommended that both methods be made official, final action.


2014 ◽  
Vol 97 (2) ◽  
pp. 498-505 ◽  
Author(s):  
Steve Kupina ◽  
Mark Roman ◽  
D Anderson ◽  
S Bhandari ◽  
M S Cardozo ◽  
...  

Abstract An international collaborative study was conducted of an HPLC-refractive index (RI) detector method for the determination of the combined amounts of sugars, glycerol, organic acids, and phenolic compounds in wines and wine-like beverages. Nine collaboratinglaboratories representing major winery, contract laboratories, and government laboratories tested eight different materials as blind duplicates using the proposed method. Sample materials included red and white wines, port, wine cooler, and nonalcoholic wine. One material was a negative control, and one material was a reference material. Samples were either treated with an ion-exchange resin to remove interferingorganic acids prior to analysis or left untreated toinclude organic acids and phenolics. Red wine samples were treated with polyvinylpolypyrrolidone to remove potential interferences from phenolics prior to analysis. The HPLC analyses were performed on a Bio-Rad Fast Acid Analysis Column using RI detection. Reproducibility (RSDR) for untreated samples(sugars + phenolics + organic acids) ranged from 6.6% for Titrivin AA4 reference material to 11.0% for dry red wine. RSDR for treated samples (sugars only) ranged from 6.8% for white zinfandel to 18.9% for dry white wine. RSDR for treatedsamples (sugars only) + glycerol ranged from 6.4% for white zinfandel to 19.8% for dry red wine. Based on these results, the method was adopted as Official First Action status for determination of total carbohydrates in wine and wine-like beverages.


1978 ◽  
Vol 24 (9) ◽  
pp. 1576-1577 ◽  
Author(s):  
R B Friedman ◽  
M A Williams ◽  
H W Moser ◽  
E H Kolodny

Abstract An improved thin-layer chromatographic method is described for the facile separation of neutral oligosaccharides excreted in the urine of patients with mannosidosis. The urine sample is treated with mixed-bed ion-exchange resin to remove charged species. The eluate is then chromatographed on silica gel thin-layer plates with n-propanol water as the developer. Eleven unique orcinol-positive components can thus be resolved. The advantages of this method over previously described techniques are the ease and rapidity of assay, better resolution of components, and clarity of resolution. It should be applicable to other disease states in which distinctive neutral carbohydrate products are produced.


1959 ◽  
Vol 37 (3) ◽  
pp. 405-416 ◽  
Author(s):  
Strathearn Wilson ◽  
David B. Smith

Horse globin has been fractionated into two components by stepwise addition of acid acetone to an acidified globin solution and by gradient elution with urea from a carboxylic-type ion exchange resin at low pH.The components obtained by both methods are similar to those prepared earlier by electrophoresis. They have similar molecular weights (about 16,000) and appear to be present in nearly equal amounts. One has the N-terminal sequence valyl-leucyl- and the other valyl-glutamyl-. They differ electrokinetically and in other properties.


2015 ◽  
Vol 2015 ◽  
pp. 1-7 ◽  
Author(s):  
Sohrabali Ghorbanian ◽  
Mostafa Davoudinejad ◽  
Amir Khakpay ◽  
Saeidreza Radpour

Breakthrough curves for citric acid adsorption from aqueous solution onto ion-exchange resin at 20, 35, and 55°C have been investigated. To predict breakthrough curves, three mathematical models have been analyzed based on the values of the least square method parameters, Durbin-Watson test, and mean relative percent error and, finally, appropriate models have been achieved. Models are in good agreement with experimental data based on the results. To examine models reliabilities and accuracy, models have been compared by various breakthrough curve data obtained by other investigators. The results show appropriate agreement and in some cases regression errors have been reduced to less than 1.0 percent.


1959 ◽  
Vol 37 (1) ◽  
pp. 405-416 ◽  
Author(s):  
Strathearn Wilson ◽  
David B. Smith

Horse globin has been fractionated into two components by stepwise addition of acid acetone to an acidified globin solution and by gradient elution with urea from a carboxylic-type ion exchange resin at low pH.The components obtained by both methods are similar to those prepared earlier by electrophoresis. They have similar molecular weights (about 16,000) and appear to be present in nearly equal amounts. One has the N-terminal sequence valyl-leucyl- and the other valyl-glutamyl-. They differ electrokinetically and in other properties.


Author(s):  
N Patel ◽  
S Patel

Empaglifozin is a Sodium-glucose co-transporter-2 inhibitors work by inhibiting SGLT2, to prevent reabsorption of glucose and facilitate its excretion in urine. Impurities in pharmaceuticals which are unwanted chemicals that remain with the active pharmaceutical ingredients (APIs), or develop during stability testing, or develop during formulation or upon aging of both API and formulation. A simple and very sensitive method developed for estimation of impurities present in Empaglifozin formulation by Reverse Phase High Performance Liquid Chromatographic method. Method is capable to detect impurities in very low level (1µg/mL). Chromatographic separation of six different impurities was achieved on Inertsil ODS-2 (250 x 4.6) mm, 3µm column using gradient elution method at 30°C column temperature and the detection was carried at 230nm at a flow rate of 1.0 mL/min. The method was validated as per ICH Q2(R1) guideline along with stress studies.


1994 ◽  
Vol 30 (12) ◽  
pp. 433-442 ◽  
Author(s):  
Alberto Cohen ◽  
Jürgen H Thiele ◽  
J. Gregory Zeikus

An experimental system was set up to study the Substrate Shuttle Process (SSP). Whey was fed to an acidogenic UASB reactor. The effluent was intermittently circulated through an Ion Exchange Unit (IEU) containing an anionic exchange resin. During a load cycle, organic acids were adsorbed onto the ion exchange resin. After completion of the load cycle, the ion exchange resin was regenerated by recirculating through it the effluent of a methanogenic UASB reactor, into which the organic acids were released, prior to returning the liquid into the reactor. The pilot system was designed to operate automatically with two IEUs operating in tandem, of which one at a time was operating in a load cycle, while the other was being regenerated. The first experimental period lasted 9 days with a cycle duration of one hour. Acids were removed from the acid UASB liquor, with a concomitant rise of pH and the production of methane in the methanogenic UASB. The acid UASB produced little gas and no methane was detected. The amount of acids circulated through the IEUs was directly proportional with the quantity of methane produced by the methane UASB. After the trial, acid binding capacity had declined to 70% of its original value. A second experiment lasted 118 days, with a cycle duration of five hours. Final conversion of all acid circulated through the IEUs into methane averaged 19%. After initial conditioning of the resin, no significant long-term deterioration of process performance was evident.


1963 ◽  
Vol 46 (3) ◽  
pp. 365-371 ◽  
Author(s):  
David Jorysch

Abstract The gradient elution technique has been applied to the investigation of organic acids present in fruit juices. In this technique, fruit juices are placed on columns containing Dowex ion exchange Resin, 1-X10, soluble fruit solids other than acids are eluted with water, and the acids are eluted with formic acid. Recovery data are given and evaluated on a number of fruit juices. Gradient elution chromatography appears to be a valuable adjunct to present analytical methods for fruit juices. Further work is necessary to determine the constancy of values, especially with regard to the varying degrees of ripeness of the fruit at the time of picking.


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