Colorimetric and Gas-Liquid Chromatographic Determination of Atropine-Hyoscyamine and Hyoscine (Scopolamine) in Solanaceous Plants

1975 ◽  
Vol 58 (5) ◽  
pp. 884-887
Author(s):  
Mohamed S Karawya ◽  
Samia M Abdel-Wahab ◽  
Mohamed S Hifnawy ◽  
Mohamed G Ghourab
Keyword(s):  
Citric Acid ◽  
Acetic Anhydride ◽  
Thin Layer ◽  
Chromatographic Determination ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Solanaceous Plants ◽  
Liquid Chromatographic ◽  
Colorimetric Methods

Abstract Two colorimetric micromethods are described for the determination of atropine-hyoscyamine and hyoscine (scopolamine), using p-dimethylaminobenzaldehyde and citric acid-acetic anhydride as the color reagents. These methods are sensitive to 60-1200 and 10-360 μg alkaloid/10 ml. The colorimetric methods were also successfully applied after a preliminary thin layer chromatographic separation of the alkaloids. A gasliquid chromatographic procedure was also developed, which yielded comparable results with the colorimetric methods.

Gas-Liquid Chromatographic Determination of Vitamin D2 in Multiple Vitamin Tablets Containing Minerals and Vitamin E Acetate

1974 ◽  
Vol 57 (5) ◽  
pp. 1089-1091
Author(s):  
David O Edlund ◽  
Florido A Filippini ◽  
James K Datson
Keyword(s):  
Vitamin E ◽  
Chromatographic Determination ◽  
Vitamin D2 ◽  
Vitamin E Acetate ◽  
Chromatographic Procedure ◽  
Ether Solution ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Column Chromatographic

Abstract A gas-liquid chromatographic procedure used to determine vitamin D2 in multiple vitamin tablets has been modified to make it applicable for analysis of multiple vitamin tablets containing minerals and vitamin E acetate. The procedure modifications involve pre-extraction with ether, solution in an alcoholic sulfuric acid-pyridine mixture, and column chromatographic separation on phosphate-treated alumina. The modified procedure has been statistically evaluated. A 2.2% coefficient of variation and 100.3% average recovery were obtained for the samples evaluated.

Reverse Phase High Performance Liquid Chromatographic Determination of Phenprocoumon in Tablets

1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Assay Procedure ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.

scholarly journals Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Maria Rambla-Alegre ◽  
Abhilasha Durgbanshi ◽  
Devasish Bose ◽  
Sandeep K. Mourya ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Cetylpyridinium Chloride ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 andN-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v)-pentanol-0.01’M NaH2PO4buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999), limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

Collaborative Study of the Gas-Liquid Chromatographic Determination of Sorbitol in Bakery Products

1973 ◽  
Vol 56 (1) ◽  
pp. 66-67
Author(s):  
Harvey K Hundley
Keyword(s):  
Aqueous Solution ◽  
Acetic Anhydride ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Bakery Products ◽  
Sugar Alcohols ◽  
Flame Ionization ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A GLC method for the determination of sorbitol has been collaboratively studied. Sugar and sugar alcohols are extracted from the bakery products by methanol and the solvent is evaporated. Acetate derivatives are then formed by addition of acetic anhydride in pyridine, and the derivatives are extracted from an aqueous solution with chloroform and analyzed by flame ionization GLC. Collaborative results show a recovery ranging from 90 to 102% sorbitol from bakery products containing 1.5 to 7% sorbitol. The method has been adopted as official first action.

scholarly journals Liquid Chromatographic Determination of Tocopherols and Tocotrienols in Vegetable Oils, Formulated Preparations, and Biscuits

2000 ◽  
Vol 83 (3) ◽  
pp. 627-634 ◽  
Author(s):  
Josep Serra Bonvehi ◽  
Francesc Ventura Coll ◽  
Imma Alsina Rius
Keyword(s):  
Vitamin E ◽  
Vegetable Oils ◽  
Chromatographic Determination ◽  
Extraction Methods ◽  
Coefficients Of Variation ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Interday Precision

Abstract A precise and selective liquid chromatographic procedure for determining tocopherol and tocotrienol isomers in vegetable oils, formulated preparations, and biscuits was developed and validated. The proposed method quantitates vitamin E in better conditions of recoverability and reproducibility than the standard saponification procedure. Tocopherols and tocotrienols were extracted in hexane from vegetable oils, passed through a silica Sep-pak, chromatographed on a μ-Bondapak C18 column with a mobile phase of methanol–water (95 + 5, v/v), identified at 292 nm, and detected with fluorescence procedure (excitation 296 nm, and emission 330 nm). The correlation coefficient on the calibration curve was 0.9995 over the range of 0.1 to 100 μg/mL. Overall recovery of vitamin E isomers was 93%; coefficients of variation for intra- and interday precision, <2.25%. The results obtained from extraction methods 1 (with saponification) and 2 (without saponification) were compared by ANOVA test. Significant differences appeared between vitamin E isomers (p ≤ 0.05).

High Pressure Liquid Chromatographic Determination of 4,4′-(Diazoamino)-dibenzenesulfonic Acid in FD&C Yellow No. 6

1977 ◽  
Vol 60 (1) ◽  
pp. 168-172
Author(s):  
Daniel M Marmion
Keyword(s):  
High Pressure ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
Liquid Chromatographic

Abstract Fourteen analysts from 9 laboratories evaluated a high pressure liquid chromatographic procedure for the determination of 4,4′-(diazoamino)-dibenzenesulfonic acid (DAADBSA) in FD&C Yellow No. 6. Each collaborator analyzed 5 samples nominally containing 0—0.050% DAADBSA. The repeatability and reproducibility of the method are estimated to be 0.003% and 0.020%, respectively. The method has been adopted as official first action.

Improvements and Modification of the Gas-Liquid Chromatographic Determination of Vitamin D2 in Multiple Vitamin Tablets and Raw Materials

1973 ◽  
Vol 56 (6) ◽  
pp. 1374-1377
Author(s):  
David O Edlund ◽  
Florido A Filippini
Keyword(s):  
Sample Preparation ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
Vitamin D2 ◽  
Column Packing ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic procedure used to determine vitamin D2 in multiple vitamin tablets and raw materials has been improved by the use of a Dexsil 300 GC column packing. Sample preparation procedures have been modified. The improved procedure has been statistically evaluated and found to be both accurate and precise.

Glucosinolates and Derived Products in Cruciferous Vegetables: Gas-Liquid Chromatographic Determination of the Aglucon Derivatives from Cabbage

1977 ◽  
Vol 60 (4) ◽  
pp. 950-953 ◽  
Author(s):  
Melvin E Daxenbichler ◽  
Cecil H VanEtten
Keyword(s):  
Enzymatic Hydrolysis ◽  
Chromatographic Determination ◽  
Cruciferous Vegetables ◽  
Internal Reference ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
The Individual ◽  
Liquid Chromatographic

Abstract A procedure is described for identifying and quantitatively determining the gīucosinolates found in edible cabbage. The intact glucosinolates are extracted and their aglucons are released into solvent after a special enzymatic hydrolysis step. The resulting isothiocyanates and oxazolidinethiones are separated by a gas-liquid chromatographic procedure that allows the individual aglucons to be identified and their amounts to be estimated by comparison with an internal reference.

Liquid-chromatographic determination of amoxapine and 8-hydroxyamoxapine in human serum.

1982 ◽  
Vol 28 (10) ◽  
pp. 2154-2157 ◽  
Author(s):  
J J Tasset ◽  
F M Hassan
Keyword(s):  
Internal Standard ◽  
Parent Drug ◽  
Chromatographic Determination ◽  
Solvent Mixture ◽  
Reversed Phase ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Toxic Concentrations ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic procedure for amoxapine and 8-hydroxyamoxapine, its active metabolite, in serum. We used a mu-Bondapak C18 reversed-phase column and a mobile phase of acetonitrile/water (74/26 by vol) plus 26 microL of n-butylamine per liter. The compounds were measured at 254 nm, with 8-methoxyloxapine as internal standard. Necessary pre-analysis purification consisted of adsorbing the drug from serum onto extraction columns, eluting with 1-butanol/hexane (1/5 by vol), re-extracting into aqueous acid, and from that re-extracting again into the elution-solvent mixture. We prefer this procedure for monitoring both therapeutic and toxic concentrations of amoxapine, because parent drug and metabolite are measured separately.

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