Liquid Chromatographic Method for Identity, Assay, and Content Uniformity of Five Tricyclic Drugs

1985 ◽  
Vol 68 (2) ◽  
pp. 168-171
Author(s):  
Edward G Lovering ◽  
Normand Beaulieu ◽  
Robert C Lawrence ◽  
Roger W Sears
Keyword(s):  
Hydrochloric Acid ◽  
Active Ingredient ◽  
Dilute Hydrochloric Acid ◽  
Chromatographic Method ◽  
Internal Standard ◽  
Peak Height ◽  
Content Uniformity ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Better Than

Abstract A liquid chromatographic (LC) procedure has been developed for the assay, content uniformity, and identification of single active ingredient solid and liquid formulations of amitriptyline, chlorpromazine, imipramine, thioridazine, and trifluoperazine. The drugs are extracted from their formulations with methanol or dilute hydrochloric acid, and identified by comparison of retention times with those of known standards; drugs are quantitated against these standards with rf/-norephedrine hydrochloride as the internal standard. The precision of replicate injections is better than 2.5% for peak area and better than 1% for peak height. The precision of triplicate determinations of tablet composites is better than 2.2%.

Liquid Chromatographic Determination of Identity, Content, and Content Uniformity of Desipramine, Fluphenazine, and Promazine

1986 ◽  
Vol 69 (1) ◽  
pp. 178-179 ◽  
Author(s):  
Normand Beaulieu ◽  
Charles Gagné ◽  
Edward G Lovering
Keyword(s):  
Hydrochloric Acid ◽  
Active Ingredient ◽  
Dilute Hydrochloric Acid ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Content Uniformity ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic procedure has been developed for the assay, content uniformity, and identification of single active ingredient formulations of desipramine, fluphenazine, and promazine. The drugs are extracted from formulations with methanol or dilute hydrochloric acid and quantitated against an internal standard (norephedrine). The drugs are identified by comparison of retention times with those of the reference standards.

Modification of the AOAC Gas-Liquid Chromatographic Method for Indole in Shrimp: Collaborative Study

1982 ◽  
Vol 65 (4) ◽  
pp. 842-845
Author(s):  
Theodore L Chambers ◽  
◽  
E C Netz ◽  
K Ogger
Keyword(s):  
Silica Gel ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Current Method ◽  
Peak Height ◽  
Modified Method ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract Several changes were suggested for standardization of the AOAC official final action gas chromatographic method for the determination of indole in shrimp. In a collaborative study, 3 FDA laboratories compared the modified method with the current method. At a 95% confidence level, the same results were obtained for each respective sample by the AOAC or the modified method, which had the following changes. The cleanup column was standardized by drying the silica gel for 2 h at 125°C and equilibrating with 3 g of water/25 g of silica gel. Concentrated ethyl acetate shrimp extracts were treated with anhydrous sodium sulfate before column cleanup and indole was eluted from the column with 15% ethyl ether/hexane. A reduced amount of the internal standard, 2-methylindole, was used to improve peak height measurements at the 25 μg% indole level. The modified method has been adopted official first action to replace method 18.075.

Gas-Liquid Chromatographic Method for Analysis of Pentachloronitrobenzene Formulations: Collaborative Study

1982 ◽  
Vol 65 (1) ◽  
pp. 110-114
Author(s):  
Alan R Hanks
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Matched Pairs ◽  
Commercial Products ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Wettable Powder ◽  
Liquid Chromatographic

Abstract A collaborative study has been conducted on a gasliquid chromatographic (GLC) method for determining pentachloronitrobenzene (PCNB) in formulations. Wettable powder, liquid, and granular matched pairs of commercial products were analyzed by 17 laboratories using peak height measurements and by 12 laboratories using integrator area measurements. Samples were dissolved in chloroform and aliquots were mixed with internal standard before GLC analysis on a 5% SE-30 column. Mean coefficients of variation for the completed study were 1.54% for integrator area measurements and 1.35% for peak height measurements. The method has been adopted official first action.

Gas-chromatographic determination of mephenytoin and desmethylmephenytoin, after off-column alkylation.

1979 ◽  
Vol 25 (1) ◽  
pp. 172-175
Author(s):  
V A Raisys ◽  
A M Zebelman ◽  
S F MacMillan
Keyword(s):  
Active Metabolite ◽  
Chromatographic Method ◽  
Seizure Control ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Therapeutic Concentration ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract We describe a gas-liquid chromatographic method for determining mephenytoin and its active metabolite, desmethylmephenytoin, in human serum. 5-Methyl-5-phenylhydantoin is used as the internal standard. The method involves extraction of the drugs by adsorption onto charcoal and off-column derivatization to their pentyl derivatives. Peak height and concentration are linearly related and the day-to-day CV for therapeutic concentration is about 2 to 6%. No interferences by endogenous compounds or drugs commonly used for seizure control have been encountered.

Collaborative Study of a Gas-Liquid Chromatographic Method for the Analysis of Chlorobenzilate and Chloropropylate

1975 ◽  
Vol 58 (3) ◽  
pp. 516-519
Author(s):  
Arthur H Hofberg ◽  
Lee C Heinrichs ◽  
Gene A Gentry
Keyword(s):  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Matched Pair ◽  
Flame Ionization ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method for the determination of chlorobenzilate and chloropropylate in liquid formulations containing about 46 and 26% active ingredient, respectively, was collaboratively studied, using a matched pair scheme. The samples were dissolved in acetone containing dibenzyl succinate as an internal standard and chromatographed on Carbowax 20M, using a flame ionization detector. Analyses of 4 samples by 13 collaborators using peak height measurements showed the following results: chlorobenzilate—2.5% overall coefficient of variation, 1.0% coefficient of variation for the random error; and 0.7% systematic error; chloropropylate—2.0, 1.4, and 0.4%, respectively. The method has been adopted as official first action.

Gas-Liquid Chromatographic Determination of Pentachloronitrobenzene in Pesticide Formulations

1976 ◽  
Vol 59 (3) ◽  
pp. 708-710
Author(s):  
Alan R Hanks ◽  
Christine W Cramer
Keyword(s):  
Chromatographic Method ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Liquid Chromatographic Method ◽  
Pesticide Formulations ◽  
Liquid Chromatographic Determination ◽  
Standard Solution ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method has been developed to determine pentachloronitrobenzene (PCNB) in pesticide formulations including dusts, powders, granules, liquids, and fertilizers. Captan, disulfoton, and Terrazole do not interfere. Samples are extracted with chloroform, and an aliquot is mixed with an equal volume of internal standard solution containing o-terphenyl. PCNB is chromatographed on a 5% SE-30 column and quantitated by peak height ratios. The method has been subjected to a ruggedness test which indicates little sensitivity to changes in extraction and chromatographic conditions.

Liquid Chromatographic Method for Determination of Azinphos-Methyl in Formulated Products: Collaborative Study

1988 ◽  
Vol 71 (5) ◽  
pp. 988-990
Author(s):  
Stephen C Slahck
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Azinphos Methyl ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Wettable Powder ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for determination of azinphosmethyl (Guthion®) in formulated products has been developed. Samples are dissolved in acetonitrile and analyzed by reverse-phase chromatography using n-butyrophenone as an internal standard. The method was subjected to a collaborative study involving 15 participating laboratories. Each collaborator was furnished with reference standard, internal standard, and blind duplicate samples of Guthion 50% wettable powder (50WP), 3 flowable (3F), and emulsifiable concentrate (2L and 2S) formulations. Collaborators were instructed to evaluate the method by peak height measurements only. Relative standard deviations for reproducibility (RSDR) were 1.11, 6.28, 2.47, and 1.17% for the 50WP, 3F, 2L, and 2S formulations, respectively. The method has been approved interim official first action for determination of azinphos-methyl in the 50WP, 2L, and 2S formulations.

Collaborative Study of a Gas-Liquid Chromatographic Method for the Analysis of Propazine

1975 ◽  
Vol 58 (3) ◽  
pp. 513-515
Author(s):  
Arthur H Hofberg ◽  
Lee C Heinrichs ◽  
Gene A Gentry
Keyword(s):  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Matched Pair ◽  
Flame Ionization ◽  
Liquid Chromatographic Method ◽  
Two Samples ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method for the determination of propazine in wettable powder formulations containing about 80% active ingredient was collaboratively studied, using a matched pair scheme. The propazine was extracted from the powder with chloroform, with dieldrin as an internal standard, and chromatographed on Carbowax 20M, using a flame ionization detector. Two samples were analyzed using peak height measurements with the following results (13 collaborators): 1.2% overall coefficient of variation and 1.2% coefficient of variation for the random error. Statistical evaluation of these factors reveals no evidence of systematic error contribution. The method has been adopted as official first action.

Liquid Chromatographic Method for Determination of Anilazine in Formulated Products: Collaborative Study

1988 ◽  
Vol 71 (1) ◽  
pp. 23-26
Author(s):  
Stephen C Slahck ◽  
◽  
J Arruda ◽  
O O Bennett ◽  
H Cheuk ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Measurement Techniques ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Liquid Chromatographic Method ◽  
Wettable Powder ◽  
Powder Samples ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the determination of anilazine (DYRENE®) in formulated products has been developed and subjected to a collaborative study involving 15 participating laboratories. Each collaborator was furnished with reference standard, internal standard, and blind duplicate samples of DYRENE 80% concentrate, 75% wettable powder (75 WP), 50 WP, and 4 flowable formulation. Samples are dissolved in acetonitrile and analyzed by reverse phase chromatography using octanophenone as an internal standard. Collaborators were instructed to evaluate the method by either peak area or peak height measurements. Seven laboratories performed the analyses using peak areas; 8 laboratories used peak heights. Peak area measurements for the wettable powder samples resulted in statistically high bias vs peak height measurements. This was apparently due to inconsistent integration parameters among collaborators. Difficulties in establishing the correct integration parameters are illustrated along with t-test values for the 2 measurement techniques. Coefficients of variation of the peak height values obtained on the 80 concentrate, 75 WP, 50 WP, and 4 flowable were 1.68,1.29,1.74, 1.87%, respectively. The method has been adopted official first action.

Comparison of a Commercial Enzymic Kit for Urinary Oxalate Analysis with a High Performance Liquid Chromatographic Method

1993 ◽  
Vol 30 (2) ◽  
pp. 186-190 ◽  
Author(s):  
Bryan J Starkey ◽  
Ian D R Fry
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Urinary Calcium ◽  
Urinary Oxalate ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Significant Interference ◽  
Better Than

A new commercial enzymic kit for urinary oxalate determination has been adapted for use on a centrifugal analyser. It has been evaluated and compared with an established high performance liquid chromatographic (HPLC) procedure developed in our laboratory. Mean recovery of oxalate from urine samples augmented with oxalic acid exceeded 97% by both methods. The precision of the HPLC method was superior to that of the enzymic kit but both methods gave between batch precision values better than CV 12% at low (less than 100μmol/L) oxalate concentrations and better than CV 7% at higher concentrations (greater than 270μmol/L) Urinary oxalate values obtained with the new enzymic procedure correlated more closely with HPLC values ( r = 0·84) than did values previously obtained using the forerunner of the kit ( r = 0·62) which was known to be susceptible to ascorbate interference. No significant interference from ascorbic acid or from high urinary calcium concentrations could be demonstrated using either the improved kit or the HPLC procedure. Its easy adaptation to automated analysers available in most laboratories, coupled to its acceptable analytical performance render the enzymic kit a reasonable alternative to HPLC or other more complex procedures for urinary oxalate analysis.

Sign in / Sign up

Export Citation Format

Share Document