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

1986 ◽  
Vol 69 (5) ◽  
pp. 915-918
Author(s):  
Edward J Kikta ◽  
◽  
E Bane ◽  
A Burns ◽  
A Christensen ◽  
...  

Abstract A liquid chromatographic (LC) method for the analysis of technical and formulated carbofuran samples was evaluated in a collaborative study. Carbofuran is determined by reverse phase LC, using a water-methanol mobile phase and acetophenone as internal standard, and detected at 280 nm. Twelve samples, 5 formulations and technical matched pairs, were analyzed by 17 collaborating laboratories. Accuracy and variability of results are typical of large LC data sets. The method has been adopted official first action.

1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted official first action.


1984 ◽  
Vol 67 (3) ◽  
pp. 492-493
Author(s):  
Stephen C Slahck ◽  
◽  
A A Carlstrom ◽  
L T Chenery ◽  
N D Ellis ◽  
...  

Abstract An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. The method has been adopted official first action.


1984 ◽  
Vol 67 (3) ◽  
pp. 497-499
Author(s):  
Stephen C Slahck ◽  
◽  
J B Audino ◽  
O O Bennett ◽  
B D Folsom ◽  
...  

Abstract A liquid chromatographic method for the determination of propoxur in technical and formulated products has been subjected to a collaborative study with 8 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with n-butyrophenone as an internal standard. Collaborators were furnished with samples of technical, 70% wettable powder, 1.5 emulsifiable, and 2% bait. Coefficient of variation values obtained on the 4 samples were 0.34, 0.68, 3.25, and 5.41%, respectively. The method has been adopted official first action.


1982 ◽  
Vol 65 (1) ◽  
pp. 132-137
Author(s):  
Norlin W Tymes ◽  
◽  
G Briguglio ◽  
C Corcoran ◽  
R Everett ◽  
...  

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.


1985 ◽  
Vol 68 (3) ◽  
pp. 567-569 ◽  
Author(s):  
Stephen C Slahck

Abstract An LC method for determination of aminocarb (Matacil™) in aminocarb technical and formulated products has been developed and subjected to a collaborative study with 10 participating collaborators. Formulations are extracted with tetrahydrofuran-buffer (60 + 40) and analyzed by reverse phase chromatography, with n-butyrophenone as internal standard. Collaborators were furnished with standards and samples of technical and 180 oil flowable products for analysis. Coefficients of variation obtained on these samples were 0.72 and 1.7%, respectively. The method has been adopted official first action.


1990 ◽  
Vol 73 (6) ◽  
pp. 893-895 ◽  
Author(s):  
Ajay G Patel ◽  
Ramanbhai B Patel ◽  
Mukeshbhai R Patel

Abstract A liquid chromatographic (LC) method has been developed for determination of clobetasone-17-butyrate In ointment using clobetasone propionate as an internal standard. Separation was carried out on a C18 reverse-phase column using water-methanol as a mobile phase. Methylparaben and propylparaben (both sodium salt) used as preservatives did not Interfere with separation. Compounds are detected photometrically at 235 nm. Mean assay results for 0.05% commercial ointments were 100.36% (n = 5). Mean recovery of clobetasone-17-butyrate added to commercial ointment was 99.89%.


1989 ◽  
Vol 72 (4) ◽  
pp. 562-563
Author(s):  
Edward J Wojtowicz

Abstract Seven laboratories participated in a collaborative study to analyze, in duplicate, 2 synthetic formulations and 2 commercial preparations, labeled to contain 3% clioquinol. Clioquinol is determined as its nickel (II) complex by reverse-phase liquid chromatography on a phenylbonded column with a mobile phase of acetonitrile-methanol-water, containing ammonium acetate and nickel chloride. Detection is at 273 nm and diphenylamine is added as an internal standard. Mean recoveries were 99.1 and 101.1%, respectively, for the ointment and cream synthetic preparations and 96.7 and 99.7%, respectively, for the commercial ointment and cream. All results are consistent with the variability of other methods at this concentration range. The method has been approved interim official first action


1982 ◽  
Vol 65 (1) ◽  
pp. 62-65
Author(s):  
Dubravka Matešič

Abstract Supplemental methionine was extracted from a feed sample with O.IM HCI and separated by reverse phase or ion-exchange high pressure liquid chromatography and isocratic elution with KH2PO4 buffer solution as the mobile phase. Methionine was detected at 205 nm. The most reliable results were obtained by using reverse phase chromatography, 0.05M KH2PO4 buffer at pH 2.6 as mobile phase, and tyrosine as internal standard.


1984 ◽  
Vol 67 (6) ◽  
pp. 1121-1122
Author(s):  
Donald Shostak ◽  
◽  
M P Uribe ◽  
T Poplawski ◽  
T S Savage ◽  
...  

Abstract A liquid chromatographic method for the determination of allopurinolin tablets was collaboratively studied by 7 laboratories. The methoduses a C,8 reverse phase column, a 0.05M ammonium phosphate mobilephase, hypoxanthine as the internal standard, and photometric detectionat 254 nm. Collaborators were supplied with samples of 2 commercialtablets and 1 synthetic tablet powder. The mean recovery value of allopurinol from the synthetic tablet powder was 100.0%. The combinedmean coefficient of variation for all 3 types of sample analyzedwas less than 2%. The method has been adopted official first action.


1986 ◽  
Vol 69 (5) ◽  
pp. 825-826
Author(s):  
Donald Shostak ◽  
Clifford Klein

Abstract A liquid chromatographic method has been developed for determination of flucytosine in capsules. Flucytosine and p-aminobenzoic acid, the internal standard, are separated on a C18 reverse phase column using water-methanol-acetic acid mobile phase containing 1-octanesulfonic acid sodium salt. Compounds are detected photometrically at 285 nm. Mean assay results for 250 and 500 mg commercial capsules were 101.5% (n = 5) and 100.2% (n = 5) of declared, respectively. Mean recovery of flucytosine added to commercial capsules was 99.3 %.


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