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).

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.

scholarly journals Liquid Chromatographic Determination of Inositol Hexanicotinate in Formulated Preparations

1997 ◽  
Vol 80 (4) ◽  
pp. 762-766
Author(s):  
Mythili Nagarajan ◽  
Ted W Waszkuc ◽  
Jidong Sun
Keyword(s):  
Dimethyl Sulfoxide ◽  
Correlation Coefficient ◽  
Calibration Curve ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Coefficients Of Variation ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A precise and selective liquid chromatographic procedure for determining inositol hexanicotinate (IHN) in formulated preparations was developed and validated. IHN was dissolved in dimethyl sulfoxide, diluted with acetonitrile, chromatographed on a Nova-Pak C18 column with a mobile phase of water-methanol (40 + 60, v/v), and detected at 262 nm. The correlation coefficient of the calibration curve was 0.9995 over the range 0.050.15 mg/mL. Overall recovery of IHN was >97%. Coefficients of variation for intra- and interday precisions were <2%.

Simultaneous liquid-chromatographic determination of vitamin K1 and vitamin E in serum.

1989 ◽  
Vol 35 (12) ◽  
pp. 2285-2289 ◽  
Author(s):  
B E Cham ◽  
H P Roeser ◽  
T W Kamst
Keyword(s):  
Vitamin E ◽  
Human Serum ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Tocopheryl Acetate ◽  
Vitamin K1 ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a high-performance liquid chromatographic procedure for the simultaneous measurement of vitamins K1 and E in human serum. Delipidated human serum (free of vitamins K1 and E) was used to make standard solutions of these vitamins, and cetyl naphthoate and alpha-tocopheryl acetate were the internal standards for vitamin K1 and vitamin E, respectively. A simple, novel separation method utilizing liquid-liquid partition chromatography was used as a preparative "clean-up" procedure. Cetyl naphthoate and vitamin K1 (after post-column reduction) were detected by fluorescence, alpha-tocopheryl acetate and vitamin E by ultraviolet absorption. Sensitivity (detection limit) of the assay was 30 pg for vitamin K1 and 5 ng for vitamin E per injection. The method is specific, precise, and more rapid than previously described procedures. Within- and between-assay CVs were 8.1% and 12.9%, respectively, for vitamin K1; 3.5% and 6.0%, respectively, for vitamin E. Analytical recoveries of vitamins K1 and E were 80% and 93%, respectively, from serum and from delipidated serum (standards). The average neonatal serum concentration of vitamin K1 was 83 ng/L, 2.5 mg/L for vitamin E; for normolipidemic adults, the values were 343 ng/L and 7.9 mg/L, respectively, and for hyperlipidemic adults, 541 ng/L and 11.1 mg/L, respectively.

Gas-Liquid Chromatographic Determination of Mirex and Photomirex in the Presence of Poly chlorinated Biphenyls: Interlaboratory Study

1980 ◽  
Vol 63 (1) ◽  
pp. 37-42 ◽  
Author(s):  
Ross J Norstrom ◽  
Henry T Won ◽  
Micheline Van Hove Holdrinet ◽  
Patrick G Calway ◽  
Caroline D Naftel
Keyword(s):  
Chromatographic Determination ◽  
Interlaboratory Study ◽  
Gas Liquid Chromatography ◽  
Coefficients Of Variation ◽  
Fuming Nitric Acid ◽  
Liquid Chromatographic Determination ◽  
Repeatability And Reproducibility ◽  
Concentrated Sulfuric Acid ◽  
Liquid Chromatographic

Abstract Mirex and photomirex (8-monohydromirex) were separated from polychlorinated biphenyls (PCBs) and other aromatic compounds by nitration with fuming nitric acid-concentrated sulfuric acid and removal of nitro-PCBs on an alumina microcolumn; the compounds were then determined by gas-liquid chromatography. Recoveries of Mirex and photomirex were 102±8 and 104±5%, respectively, from standard solutions which had a PCB-to-Mirex and photomirex ratio of 1000. Recoveries from fortified, uncontaminated samples of sediment, fish, and eggs averaged 93±7 and 92±3% for Mirex and photomirex, respectively. The coefficients of variation for repeatability and reproducibility averaged 8 and 15%, respectively, in an interlaboratory study conducted by 4 laboratories using extracts of naturally contaminated substrates (sediment, carp, eel, and gull egg). Levels of Mirex in the samples ranged from 0.1 to 8 mg/kg, and levels of PCB ranged from 0.5 to 166 mg/kg.

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.

High Performance Liquid Chromatographic Determination of Methapyrilene Hydrochloride in Feed and Sleep Aid Tablets

1981 ◽  
Vol 64 (4) ◽  
pp. 889-892
Author(s):  
Badaruddin Shaikh ◽  
Margarette R Hallmark
Keyword(s):  
High Performance ◽  
Ammonium Carbonate ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Phase Partition ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Methapyrilene hydrochloride (MP·HCl) was extracted from feed with methanol and determined by reverse phase partition chromatography in less than 15 min, using isocratic elution with acetonitrile-1.1% ammonium carbonate (1 + 1) as the mobile phase. This procedure was tested on feed treated with MP·HCl at levels of 125,500, and 2000 ppm. Recoveries were 104,95, and 96% with coefficients of variation of 2.4,1.6, and 0.6%, respectively. MP·HCl in feed was stable for 14 days. This method was also successfully used to determine MP·HCl in 3 sleep aid tablets.

Gas-Liquid Chromatographic Determination of Tetradif on Technical and Formulations: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 829-832
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
James E Launer ◽  
◽  
E C Calamita ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic determination of tetradifon technical and formulations was collaboratively studied in duplicate with 12 laboratories. Six samples were dissolved in dichloroethane with n-hexacosane as the internal standard, chromatographed on a column of 3% SE-52, and detected by flame ionization. The average coefficients of variation were 1.2% for the 2 technical samples, 1.6% for the 2 wettable powders, and 1.5% for the 2 emulsifiable concentrates. The method has been adopted official first action.

Liquid Chromatographic Determination of Triadimefon in Technical and Formulated Products: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

Abstract A liquid chromatographic method for the determination of triadimefon (Bayleton™) in triadimefon technical and formulated products has been developed and subjected to a collaborative study with 7 participating collaborators. Formulations were extracted with mobile solvent and analyzed by normal phase chromatography, with 4-chlorophenyl sulfoxide as an internal standard. Collaborators were furnished with standards and samples of technical products, 50% wettable powders, and 25% wettable powders for analysis. Coefficients of variation of the values obtained on these samples were 1.42, 0.82, and 1.05%, respectively. The method has been adopted official first action.

Ion Pairing High Pressure Liquid Chromatographic Determination of Amaranth in Licorice Products

1981 ◽  
Vol 64 (6) ◽  
pp. 1411-1413
Author(s):  
William J Hurst ◽  
James M Mckim ◽  
Robert A Martin
Keyword(s):  
High Pressure ◽  
Ion Pairing ◽  
Chromatographic Determination ◽  
Buffer Solution ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic method is described for the determination of amaranth (FD&C Red No. 2; Red No. 2) in licorice products. The Red No. 2 is extracted with a basic buffer solution, cleaned up on a Sep-Pak column, chromatographed on a reverse phase column in the ion pairing mode, and detected at 254 nm. The procedure is time-conservative with accurate and precise results. Recovery data ranged from 93 to 104%, and coefficients of variation were less than 4% for standards and samples.

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.

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