Improved Extraction and HPLC Methods for Ergovaline from Plant Material and Rumen Fluid

1994 ◽  
Vol 6 (3) ◽  
pp. 348-352 ◽  
Author(s):  
A. Morrie Craig ◽  
Dan Bilich ◽  
Jeannette T. Hovermale ◽  
Ronald E. Welty
Keyword(s):  
Tall Fescue ◽  
Plant Material ◽  
Rumen Fluid ◽  
Accurate Diagnosis ◽  
Fescue Toxicosis ◽  
Acremonium Coenophialum ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Fast Analysis ◽  
Liquid Chromatographic

Ergovaline, the main ergopeptine alkaloid produced in tall fescue infected with Acremonium coenophialum, is known to cause tall fescue toxicosis. Current methods in use for quantifying ergovaline in plant material have several disadvantages, including large solvent volumes and long analysis time. We report here improvements in extraction and cleanup and the high-pressure liquid chromatographic methods. Our improvements include a 24-hour extraction time, the use of smaller solvent volumes during sample preparation, and fast analysis on the polymeric reverse-phase column. In addition to allowing the analysis of large batches to assist practitioners in the accurate diagnosis of fescue toxicosis, our method is also easily modified for other matrices, such as rumen fluid.

ENANTIOSELECTIVE ANALYSIS OF GUAIFENESIN IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY CHIRAL REVERSE PHASE HPLC-PDA METHOD

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 36-43
Author(s):  
B. Tharunkumar ◽  
◽  
P. Kalyani ◽  
M. Lakshmiprasanna ◽  
B. N. Nalluri
Keyword(s):  
Dosage Forms ◽  
Racemic Mixture ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Pharmaceutical Dosage Forms ◽  
Enantioselective Analysis ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A novel, accurate and precise chiral reverse-phase high pressure liquid chromatographic method was developed for enantioselective analysis of guaifenesin (GFN) in bulk and tablet dosage forms. Chiral separation was achieved on phenomenex Lux Cellulose-4 column (250×4.6mm, 5μ) using 0.02% formic acid: acetonitrile (90:10 V/V) as the mobile phase at a flow rate of 1mL/min at 230nm. The retention times of GFN enantiomers A and B was 15 and 16 minutes, respectively, with good peak resolutions and showing good linearity in the concentration range of 10-50 μg/mL (R2 > 0.999). The developed method was validated as per the International Conference on Harmonization guidelines and the results were well within the acceptable limits. The percentage assay in tablet dosage form was found to be 98.8 and 98.2 respectively, for enantiomers A and B and was with in the compendial specifications, demonstrating the suitability of developed method for enantioselective analysis of guaifenesin racemic mixture.

Preparation and Spectral Analysis of 3,3',4,4'-Tetrachloroazobenzene and the Corresponding Azoxy and Hydrazo Analogs

1979 ◽  
Vol 62 (4) ◽  
pp. 746-750
Author(s):  
M T Stephen Hsia ◽  
Charles F Burant
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Chromatographic Method ◽  
Lithium Aluminum Hydride ◽  
Aluminum Hydride ◽  
Lithium Aluminum ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Hydride Reduction ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract An efficient preparation was developed for 3,3',4,4'-tetrachloroazobenzene and the corresponding azoxy and hydrazo derivatives, based on the lithium aluminum hydride reduction of 3,4-dichIoronitrobenzene. Batches were analyzed for purity by using a reverse phase high pressure liquid chromatographic method. All 3 compounds can be synthesized in gram quantities with 97–99% purity. Detailed mass, infrared, and nuclear magnetic resonance spectral analyses are presented.

Application of Gel Permeation Chromatography and Nonaqueous Reverse Phase Chromatography to High Pressure Liquid Chromatographic Determination of Retinyl Palmitate in Fortified Breakfast Cereals

1980 ◽  
Vol 63 (1) ◽  
pp. 131-136 ◽  
Author(s):  
William O Landen
Keyword(s):  
High Pressure ◽  
Vitamin A ◽  
Methylene Chloride ◽  
Colorimetric Method ◽  
Gel Permeation Chromatography ◽  
Retinyl Palmitate ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Gel Permeation ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method was developed for determining retinyl palmitate in cereals. Retinyl palmitate is fractionated from other methylene chloride-soluble components by using high pressure gel permeation chromatography (HP-GPC) followed by quantitation with nonaqueous reverse phase HPLC (RPHPLC). HP-GPC fractionation was accomplished using 2 µStyragel (100Å) columns connected in series on sample extracts in methylene chloride with methylene chloride as the mobile phase. A valve designed to facilitate the collection of the vitamin A fraction was installed in-line between the refractive index and absorbance detectors. RPHPLC quantitation was achieved on µBondapak C18 (10 µm) using methylene chloride–acetonitrile (30+70). Based on 23 repetitive analyses, recovery of vitamin A as retinyl palmitate in cereal products was 95.4±4.2% with spiking levels between 21.4 and 140 µg/g. Vitamin A in 15 cereals, representing bran, corn, oats, rice, and wheat, ranged from 34 to 194% of the declared level. The HPLC procedure was compared with the AOAC official colorimetric method and with an ultraviolet spectrophotometric method.

High Pressure Liquid Chromatographic Determination of Oxazepam Dosage Forms: Collaborative Study

1983 ◽  
Vol 66 (4) ◽  
pp. 864-866
Author(s):  
Eileen S Bargo ◽  
◽  
E Aranda ◽  
C Bonnin ◽  
S Hauser ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A reverse phase high pressure liquid chromatographic method for the determination of oxazepam in tablets and capsules was collaboratively studied by 9 laboratories. Collaborators were supplied with 6 samples that included synthetic and commercial formulations. Tablet and capsule composites are diluted with methanol and filtered. Oxazepam is determined at 254 nm by using a C18 column. Mean recoveries of oxazepam from synthetic tablet and capsule formulations were 97.2 and 99.0%, respectively. Mean coefficients of variation for tablets and capsules ranged from 1.85 to 2.86%. The method has been adopted official first action.

High Pressure Liquid Chromatographic Determination of Physostigmine Salicylate and Physostigmine Sulfate in Liquids and Ointments: Collaborative Study

1982 ◽  
Vol 65 (1) ◽  
pp. 132-137
Author(s):  
Norlin W Tymes ◽  
◽  
G Briguglio ◽  
C Corcoran ◽  
R Everett ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Results of 11 laboratories are presented for the collaborative study of a proposed method for the quantitative reverse phase high pressure liquid chromatographic (HPLC) determination of physostigmine salicylate and physostigmine sulfate in pharmaceutical formulations. The samples consisted of commercial solution, injection, and ointment preparations, each containing one of the physostigmine salts. The physostigmine salt is extracted from ointments with acetonitrile after the ointment is dissolved in hexane. Liquid preparations are diluted directly. Physostigmine is determined at 254 nm on a C18 column by comparison with a physostigmine standard. Flurazepam hydrochloride is the internal standard. The method has been adopted official first action for the solution dosage form.

High Pressure Liquid Chromatographic Determination of Antihistamine-Adrenergic Combination Products

1980 ◽  
Vol 63 (1) ◽  
pp. 91-94 ◽  
Author(s):  
William J Bachman
Keyword(s):  
High Pressure ◽  
Liquid Chromatography ◽  
Chromatographic Determination ◽  
Step Response ◽  
Chlorpheniramine Maleate ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Reverse phase high pressure liquid chromatography (HPLC) with ion-pairing is used for the determination of pseudoephedrine hydrochloride in combination with triprolidine hydrochloride or chlorpheniramine maleate in sirups and tablets. Sirups require a preliminary column chromatography cleanup step. Response is linear for pseudoephedrine hydrochloride (range of 0–20 μg), chlorpheniramine maleate (range of 0–1.3 μg), and triprolidine hydrochloride (range of 0–1.0 μg). Recoveries from synthetic formulations were 98.8–101.3% for pseudoephedrine hydrochloride, 100.0–101.2% for chlorpheniramine maleate, and 97.7–99.8% for triprolidine hydrochloride. The coefficient of variation for the method is less than 1%.

High Pressure Liquid Chromatographic Determination of Theobromine and Caffeine in Cocoa and Chocolate Products

1978 ◽  
Vol 61 (6) ◽  
pp. 1424-1427 ◽  
Author(s):  
Wesley R Kreiser ◽  
Robert A Martin
Keyword(s):  
High Pressure ◽  
Chromatographic Determination ◽  
Hot Water ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Hot Water Extraction ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method was developed for determining theobromine and caffeine in cocoa and chocolate products by high pressure liquid chromatography. After a simple hot water extraction, both theobromine and caffeine were separated by using a reverse phase Cl s column and a mobile phase of methanol-water-acetic acid (20+ 79+1). Theobromine and caffeine were quantitated at 280 nm; average recoveries were 98.7 and 95.0%; and coefficients of variation were 2.31 and 3.91%, respectively.

High Pressure Liquid Chromatographic Separation of Rotenoids from Plant Extracts

1979 ◽  
Vol 62 (4) ◽  
pp. 774-781 ◽  
Author(s):  
Stephen E Moring ◽  
James D McChesney
Keyword(s):  
High Pressure ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Mass Spectral ◽  
Liquid Chromatographic Separation ◽  
Amorpha Canescens ◽  
Liquid Chromatographic ◽  
Chloroform Methanol ◽  
Column Chromatographic

Abstract The concomitant isolation, identification, and quantitative determination of rotenoids by high pressure liquid chromatography and ultraviolet and mass spectral analyses is presented. Plant samples are extracted with chloroform-methanol, subjected to a combination of solvent partitioning and silica gel open column chromatographic cleanup, and then chromatographed by HPLC reverse phase techniques. Concentrations of rotenone and deguelin are reported for Tephrosia virginiana (L.) Pers. and Amorpha canescens Persh.

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