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 ◽  
...  

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.

1983 ◽  
Vol 66 (4) ◽  
pp. 864-866
Author(s):  
Eileen S Bargo ◽  
◽  
E Aranda ◽  
C Bonnin ◽  
S Hauser ◽  
...  

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.


1981 ◽  
Vol 64 (6) ◽  
pp. 1411-1413
Author(s):  
William J Hurst ◽  
James M Mckim ◽  
Robert A Martin

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.


1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck

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.


1980 ◽  
Vol 63 (3) ◽  
pp. 591-594
Author(s):  
Wesley R kreiser ◽  
Robert A Martin ◽  
◽  
R Bigornia ◽  
R Bond ◽  
...  

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.


1986 ◽  
Vol 69 (5) ◽  
pp. 908-911
Author(s):  
Peter L Carter ◽  
Keith C Overton ◽  
◽  
P G Baker ◽  
O O Bennett ◽  
...  

Abstract A liquid chromatographic method for determination of bendiocarb in technical materials and wettable powders was tested by 12 collaborators. Bendiocarb is dissolved in acetonitrile containing 0.1% propiophenone as internal standard. This solution is analyzed on a liquid chromatograph utilizing a reverse phase (C18) column. The compound is detected at 254 nm and peak area is used for quantitation. The 3 different materials studied contained 20, 80, and nominally 100% bendiocarb. Each was examined in duplicate to provide the necessary matched pairs. Collaborators approved of the ease and simplicity of the method and, in particular, the way the method can be applied to automatic injection assemblies. The statistical data show acceptable precision of the method: Reproducibility coefficients of variation were 20% material, 2.04%; 80% material, 1.02%; and nominal 100% material (technical product), 0.64%. 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.


1980 ◽  
Vol 63 (1) ◽  
pp. 91-94 ◽  
Author(s):  
William J Bachman

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%.


1975 ◽  
Vol 58 (1) ◽  
pp. 48-49 ◽  
Author(s):  
Manjeet Singh

Abstract A high-pressure liquid chromatographic method is presented for the isolation and determination of uncombined intermediates and subsidiary colors in FD&C Blue No. 2 (indigotine, C.I. No. 73015). Samples of FD&C Blue No. 2 containing 0.1–0.3% isatin, 0.1–0.3% isatin 5-sulfonic acid, 0.1–5.0% monosulfonated indigo, and 1.0–18.0% 5,7’-disulfonated indigo were prepared and analyzed by using this method. Recoveries ranged between 92 and 102%.


1986 ◽  
Vol 69 (4) ◽  
pp. 594-597 ◽  
Author(s):  
Elia D Coppola ◽  
Martin S Starr ◽  
◽  
G H Chang ◽  
J DeVries ◽  
...  

Abstract Twelve laboratories collaboratively studied a liquid chromatographic method for determination of quinic, malic, and citric acids in cranberry juice cocktail and apple juice. Samples are passed through a disposable silica cartridge, filtered, and directly injected into the chromatograph. The mobile phase is 0.2M KH2PO4 (pH 2.4). Two reverse phase columns are used, with UV detection at 214 nm. Six samples of cranberry juice cocktail and 6 samples of apple juice were sent to each collaborator. Repeatability and reproducibility coefficients of variation ranged from 1.2 to 7.6% and from 2.9 to 14.7%, respectively, for quinic, malic, and citric acid levels above 0.10%. The precision of the method is satisfactory. The method has been adopted official first action.


1978 ◽  
Vol 61 (6) ◽  
pp. 1424-1427 ◽  
Author(s):  
Wesley R Kreiser ◽  
Robert A Martin

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.


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