High Pressure Liquid Chromatographic Determination of Ethion in Formulations: Collaborative Study

1979 ◽  
Vol 62 (1) ◽  
pp. 11-14
Author(s):  
James E Launer
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid high pressure liquid chromatographic (HPLC) method is described for determining ethion (O,O,O',0'-tetraethyl-S,S'-methylene bisphosphorodithioate) in formulations, using reverse phase columns of either μBondapak C18/Porasil or ODS Permaphase. The sample is dissolved in either methanol for μBondapak C18 or acetonitrile for ODS Permaphase; pentachloronitrobenzene is used as an internal standard. After inert materials are removed, the supernate is injected onto the HPLC column and the compound is quantitated by peak height ratios at 254 nm. Six collaborators made single determinations of 8 samples. The average coefficients of variation were 0.76% for the 2 technical samples, 0.63% for the two 50% formulations, 0.95% for the two 25% wettable powders, and 0.76% for the two 2% oil formulations. The method was adopted as official first action.

High Pressure Liquid Chromatographic Method for Indole in Shrimp: Development of Method and Collaborative Study

1981 ◽  
Vol 64 (3) ◽  
pp. 592-602 ◽  
Author(s):  
Theodore L Chambers ◽  
Walter F Staruszkiewicz ◽  
◽  
G Bohm ◽  
J F Bond ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Hplc Method ◽  
Fluorescence Detector ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Spectrofluorometric Method ◽  
Liquid Chromatographic

Abstract A collaborative study on the determination of indole in shrimp was conducted in which a high pressure liquid chromatographic (HPLC) method and a spectrofluorometric method were compared with the AOAC gas-liquid chromatographic (GLC) method (18.075–18.078,13th ed.). In the HPLC method, 10 g shrimp was blended with methanol, an internal standard was added, and the extract was filtered. Indole was separated on an octadecylsilane reverse phase column, using 60% MeOH-H2O, and quantitated with a fluorescence detector (excitation 280 nm, emission 330 nm) by comparing the indole peak height with that of an internal standard, 2-methylindole. Recoveries at a 25 μg/100 g level averaged 104% with a range of 90–127%, and at a level of 35 μg/100 g averaged 102% with a range of 93–112%. In the spectrofluorometric method, 25 g shrimp was extracted with 2% EtOAc-hexane. After several washes, indole was partitioned into a saturated NaCl-MeOH solution and its fluorescence was measured (excitation 280 nm, emission 332 nm). Recoveries at a 25 μg/100 g level averaged 93% with a range of 0–255% and at a level of 35 μg/100 g averaged 64% with a range of 0–107%. Recoveries obtained by the AOAC-GLC method at a level of 25 μg/100 g averaged 96% with a range of 81–116% and at a level of 35 μg/100 g averaged 101% with a range of 81–119%. The coefficients of variation were 20,10, and 64% at a 25 μg/100 g level for the GLC method, the HPLC method, and the spectrofluorometric method, respectively. The HPLC method was adopted as official first action for indole levels in shrimp exceeding 1 μg/100 g.

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

1980 ◽  
Vol 63 (3) ◽  
pp. 591-594
Author(s):  
Wesley R kreiser ◽  
Robert A Martin ◽  
◽  
R Bigornia ◽  
R Bond ◽  
...  
Keyword(s):  
High Pressure ◽  
Petroleum Ether ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Peak Height ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

Abstract Four duplicate samples of cocoa-containing materials, a practice sample, and standards were submitted to the collaborators for theobromine and caffeine analysis by HPLC. In the method the samples are defatted with petroleum ether, and dried. The fat-free residue is then extracted with water and an aliquot is injected into the chromatograph. Compounds are quantitated by comparison with internal or external standards, either by peak height or peak area. Results for all the analyses showed that few of the values were more than 2 standard deviations from the mean. The method has been adopted as official first action.

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 Ethopabate in Feeds

1977 ◽  
Vol 60 (5) ◽  
pp. 1048-1050
Author(s):  
Leonard R Schronk ◽  
Billy M Colvin ◽  
Alan R Hanks ◽  
Rodney J Bushway
Keyword(s):  
High Pressure ◽  
Limit Of Detection ◽  
Colorimetric Method ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Hplc Method ◽  
Detector Response ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) method is described for determining ethopabate in poultry feeds. Feed samples containing ethopabate are finely ground, extracted 30 min by sonification with methanol-water (80+20), and filtered. The extract is cleaned up on an alumina column, and the first 4 ml eluate collected is analyzed. The drug is eluted through a μBondapak C18 column with acetonitrile-water (30+70) at a flow rate of 1.4 ml/min and detected by ultraviolet absorption at 280 nm. Chromatography is complete in 7 min, and detector response is linear. The drug is quantitated by peak height ratios. The procedure described is reproducible and shows good agreement with the official AOAC colorimetric method. The lower limit of detection is 2 ng by HPLC, making the method applicable to residue analyses.

High Pressure Liquid Chromatographic Determination of Nitrogen Derived from Urea and Water-Soluble Methylene Ureas in Urea Formaldehyde Fertilizers: Collaborative Study

1983 ◽  
Vol 66 (3) ◽  
pp. 769-774
Author(s):  
Allan D Davidson ◽  
◽  
E R Austin ◽  
B M Christensen ◽  
D Coggin ◽  
...  
Keyword(s):  
High Pressure ◽  
Urea Formaldehyde ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Water Soluble ◽  
High Pressure Liquid Chromatographic ◽  
Paired Samples ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A melhod for measuring nitrogen derived from urea, melhylenediurea (MDU), and dimethylenetriurea (DMTU) was tested by 9 collaborators. Collaborators made single determinations on 2 separate days on 5 sets of paired samples. Samples were extracted with water, filtered, and analyzed after high pressure liquid chromatographic separation on a C-8 or C-18 bonded silica column, using a refractive index detector. Peak heights compared to external standard of each component were used for quantitation. Mean coefficients of variation for the completed study were 3.24% for urea, 3.48% for MDU, and 6.56% for DMTU. The method has been adopted official first action.

High Pressure Liquid Chromatographic Determination of Phenol in Honey

1981 ◽  
Vol 64 (2) ◽  
pp. 337-339
Author(s):  
Peter Sporns
Keyword(s):  
High Pressure ◽  
Mobile Phase ◽  
Silicic Acid Column ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is described for determining phenol in honey by using high pressure liquid chromatography (HPLC). An internal standard, 2-phenylethanol, was added to honey which was steam-distilled and chromatographed on a 25 cm × 3.2 mm id Spherisorb 5 µm silicic acid column using water as the mobile phase. Absorbance was monitored at 195 nm. Using a mixed standard of known concentration and peak height measurements, the amount of phenol in the honey could be quantitated. Recovery of added phenol was checked at levels from 0.1 to 33 ppm.

High Pressure Liquid Chromatographic Determination of Antihistamine-Adrenergic Combination Products: Collaborative Study

1981 ◽  
Vol 64 (3) ◽  
pp. 564-569 ◽  
Author(s):  
William J Bachman ◽  
◽  
M Y Alpert ◽  
E Bargo ◽  
R E Draper ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Chlorpheniramine Maleate ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A reverse phase high pressure liquid chromatographic method in which ion-pairing is used for the determination of combinations of pseudoephedrine hydrochloride with triprolidine hydrochloride or chlorpheniramine maleate in syrups and tablets was collaboratively studied by 8 laboratories. Collaborators were supplied with 12 samples including synthetic and commercial syrup formulations and commercial tablet composites. Mean recoveries of pseudoephedrine hydrochloride and triprolidine hydrochloride from synthetic syrup formulations were 100.5 and 99.6%, respectively. Mean recoveries of pseudoephedrine hydrochloride and chlorpheniramine maleate from synthetic syrups were 98.8 and 100.5%, respectively. Mean coefficients of variation for syrups and tablets ranged from 1.68 to 3.07% for pseudoephedrine hydrochloride, from 2.92 to 3.85% for triprolidine hydrochloride, and from 1.34 to 2.15% for chlorpheniramine maleate. The method has been adopted official first action.

High Pressure Liquid Chromatographic Determination of Monoand Disaccharides in Presweetened Cereals: Collaborative Study

1982 ◽  
Vol 65 (2) ◽  
pp. 256-264 ◽  
Author(s):  
Lucian C Zygmunt ◽  
◽  
E Anderson ◽  
B Behrens ◽  
R Bowers ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Water Alcohol

Abstract A collaborative study was conducted using a modified AOAC method (sugars in chocolate) for the determination of fructose, glucose, sucrose, and maltose in presweetened cereals by high pressure liquid chromatography (HPLC). Eight samples consisting of 6 products were analyzed in duplicate by the HPLC method and the AOAC Lane-Eynon method. The AOAC method was modified to use water-alcohol (1 + 1) and Sep-Pak C18 cartridges for sample cleanup. The HPLC results indicate precision comparable to the Lane-Eynon method and the chocolate method. The modified HPLC method has been adopted official first action.

Isomer Specific Assay of Ester and Salt Formulations of 2,4-Dichlorophenoxyacetic Acid by High Pressure Liquid Chromatography: Collaborative Study

1978 ◽  
Vol 61 (5) ◽  
pp. 1163-1165 ◽  
Author(s):  
Timothy S Stevens ◽  
Norman E Skelly ◽  
Robert B Grorud
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Internal Standard ◽  
Dichlorophenoxyacetic Acid ◽  
High Pressure Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Standard Solution ◽  
2,4 Dichlorophenoxyacetic Acid ◽  
Liquid Chromatographic

Abstract A high pressure liquid chromatographic (HPLC) assay of ester and salt formulations of 2,4-D has been collaboratively studied. The method is specific for 2,4-D isomer and resolves all known impurities from 2,4-D and the internal standard p-bromophenol. In situ saponification, at room temperature, is performed by adding a combined saponification-internal standard solution to ester products. The same saponification- internal standard solution is added to amine salts and the analytical standard. The injected aqueous potassium salt solution of 2,4-D is then converted to the acid form by an acidic buffered mobile solvent of 20% acetonitrile in water. Optimum chromatography is attained by a mobile solvent pH of 2.95 in a reverse phase microparticulate column, by ion suppression. Each of the 9 collaborators received 3 different ester and 2 different amine formulations of 2,4-D. The coefficients of variation of 2,4-D acid equivalent ranged from 1.22 to 1.59%. The method has been adopted as official first action.

Sign in / Sign up

Export Citation Format

Share Document