Gas-Liquid Chromatographic Determination of Pyridazinones in Technical Products and Formulations

1978 ◽  
Vol 61 (1) ◽  
pp. 161-163
Author(s):  
Giuseppe Cellerino ◽  
Mariarosa Re
Keyword(s):  
Internal Standard ◽  
Standard Technique ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Selective Detector ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

Abstract Simultaneous determination of the active ingredient and of by-products in technical and formulated pyridazinones was rapidly performed by gas-liquid chromatography with complete resolution of all compounds. Quantitative determination by the internal standard technique is accurate and precise. The lower limit of detectability is 8 × 10–12 g/sec with a flame ionization detector and 1 × 10–12 g/sec with a nitrogen-phosphorus selective detector operating in the nitrogen mode.

Gas-Liquid Chromatographic Determination of p-Chloroacetanilide in Acetaminophen

1978 ◽  
Vol 61 (1) ◽  
pp. 68-71
Author(s):  
Dorothy K Wyatt ◽  
Lee T Grady
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Flame Ionization ◽  
Glass Column ◽  
Retention Characteristics ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Gas-liquid chromatography (GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m × 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10–100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.

Gas-Liquid Chromatographic Determination of Paraldehyde in Paraldehyde Elixir

1972 ◽  
Vol 55 (1) ◽  
pp. 166-169
Author(s):  
William T Lampkin
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Standard Technique ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Glass Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A collaborative study was conducted on a GLC method for determining paraldehyde in pharmaceutical preparations of paraldehyde elixirs. Eleven collaborating laboratories analyzed 2 unknown paraldehyde solutions and a solution of known paraldehyde concentration. Recoveries of 15–25% paraldehyde solutions averaged 98.5% with a coefficient of variation of about 2%. The method consists of diluting a sample aliquot to a definite volume and determining the paraldehyde content by GLC, using a flame ionization detector and a 6’ × 4 mm coiled glass column packed with 80–100 mesh Diatoport S coated with 2% HIEFF-8BP (cyclohexane dimethanol succinate) plus 20% Carbowax 20M. The internal standard technique was used for calculation. It is recommended that the method be adopted as official first action.

Gas-Liquid Chromatographic Determination of Tetradif on Technical and Formulations: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 829-832
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
James E Launer ◽  
◽  
E C Calamita ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic determination of tetradifon technical and formulations was collaboratively studied in duplicate with 12 laboratories. Six samples were dissolved in dichloroethane with n-hexacosane as the internal standard, chromatographed on a column of 3% SE-52, and detected by flame ionization. The average coefficients of variation were 1.2% for the 2 technical samples, 1.6% for the 2 wettable powders, and 1.5% for the 2 emulsifiable concentrates. The method has been adopted official first action.

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

1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

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.

Liquid Chromatographic Determination of Carbamazepine in Tablets

1988 ◽  
Vol 71 (3) ◽  
pp. 523-525 ◽  
Author(s):  
Ella S Walker
Keyword(s):  
Internal Standard ◽  
Standard Technique ◽  
Chromatographic Determination ◽  
Individual Values ◽  
Qualitative And Quantitative ◽  
Average Value ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid liquid chromatographic method is described for the qualitative and quantitative determination of carbamazepine in tablet composites and individual tablets, using the internal standard technique. Analyses were performed on a C-18 reverse-phase column with tetrahydrofuran-methanol-water (8 + 37 + 55) as the mobile phase. A linear relationship was obtained between detector responses at 254 nm and amounts of carbamazepine injected ranging from 0.2 to 1.7 ng. The coefficient of variation for 10 consecutive injections of a standard preparation was 0.4%. Recoveries of carbamazepine from 100 and 200 mg tablets averaged 101.4 and 99.7%, respectively. Assay results for commercial tablets analyzed by the proposed method agreed favorably with those obtained by the method of USP XXI. The assay results for individual tablets indicated that deviations from the average value and the range of individual values are much wider with the compendial method than with the proposed method

Gas-Liquid Chromatographic Determination of β-Asarone in Wines and Flavors

1976 ◽  
Vol 59 (3) ◽  
pp. 675-677
Author(s):  
Randolph H Dyer ◽  
Glenn E Martin ◽  
Peter C Buscemi
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Ethyl Palmitate ◽  
Ultraviolet Spectra ◽  
Liquid Chromatographic Determination ◽  
Mass Spectrometery ◽  
Liquid Chromatographic

Abstract Wine samples containing β-asarone (cis-2,4,5-trimethoxy-1-propenylbenzene) are distilled; β-asarone is extracted by hexane and then quantitatively determined by gas-liquid chromatography (GLC), using ethyl palmitate as the internal standard. The GLC procedure is rapid and yields precise and accurate results. Mass spectrometery confirmed the identity of the GLC peak as β-asarone. The ultraviolet spectra of β-asarone and its isomer were also determined.

Gas-Liquid Chromatographic Determination of Isosorbide Dinitrate in Tablets

1977 ◽  
Vol 60 (6) ◽  
pp. 1341-1344
Author(s):  
David G Prue ◽  
Raymond N Johnson ◽  
Boen T Kho
Keyword(s):  
Isosorbide Dinitrate ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Phase System ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic (GLC) method is described for determining isosorbide dinitrate (ISDN) in tablets. ISDN is extracted from tablet excipients by a 2-phase system composed of water-ethyl ether, and detected and quantitated with a flame ionization detector after separation from the internal standard (glyceryl tributyrate) on a 3% OV-210 column. Ten replicate assays on 2 different batches of tablets, each containing 5 mg ISDN, gave coefficients of variation of 1.16 and 1.48%, respectively. Comparison of results obtained for tablets containing 5, 10, and 40 mg ISDN, and for diluted isosorbide dinitrate raw material containing 25% ISDN, showed good correlation among the GLC, USP colorimetric, and USP polarographic procedures. Assay of synthetic mixtures containing ISDN, isosorbide-2-mononitrate, and isosorbide-5-mononitrate demonstrated that the GLC procedure is specific for ISDN, whereas the USP polarographic procedure is subject to interference from the mononitrates.

Multiple Internal Standard Technique for the Gas-Liquid Chromatographic Determination of Indole in Shrimp

1978 ◽  
Vol 61 (1) ◽  
pp. 136-138
Author(s):  
Walter F Staruszkiewicz ◽  
John F Bond
Keyword(s):  
Silica Gel ◽  
Room Temperature ◽  
Internal Standard ◽  
Standard Technique ◽  
Chromatographic Determination ◽  
Experimental Conditions ◽  
Liquid Chromatographic Determination ◽  
Standard Solution ◽  
Liquid Chromatographic

Abstract A multiple internal standard technique has been developed for the official first action gas-liquid chromatographic (GLC) method for determining indole in shrimp. The modification was developed because interfering GLC peaks are occasionally observed when 2-methylindole is used as the internal standard. An internal standard solution containing 1-methylindole, 2- methylindole, and diphenylamine was added to extracts of shrimp before silica gel cleanup and separation by GLC. All of the compounds were quantitatively recovered and were separated on the GLC column under identical experimental conditions. Extracts of acceptable shrimp to which indole was added at levels of 3–10 μg/ 100 g and extracts of decomposed shrimp were stored at room temperature for 2 weeks. Average and maximum changes (μg indole/100 g) during storage were, respectively, for each internal standard: average 0.6, 0.4, and 1.1; maximum 1.7, 0.9, and 2.9.

Collaborative Study of Gas-Liquid Chromatographic Determination of Methaqualone in Pharmaceutical and Clandestine Preparations

1977 ◽  
Vol 60 (4) ◽  
pp. 935-939 ◽  
Author(s):  
Harold F Hanel
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Eight laboratories collaboratively studied a procedure for the quantitative determination of methaqualone. HCl in pharmaceutical and clandestine preparations. Methaqualone is extracted from an aqueous bicarbonate solution into chloroform and quantitated by gas-liquid chromatography on a 3% OV-1 column. Tetraphenylethylene is used as an internal standard. Two commercial preparations and 4 sample mixtures prepared by the author were studied. Recoveries for the 4 prepared samples ranged from 100.0 to 102.6%, and the coefficients of variation ranged from 1.58 to 4.15% for the 6 samples studied. The method has been adopted as official first action.

Gas-Liquid Chromatographic Determination of Aniline Metabolites of Substituted Urea and Carbamate Herbicides in Aqueous Solution

1981 ◽  
Vol 64 (4) ◽  
pp. 833-840
Author(s):  
Erika E Hargesheimer ◽  
Ronald T Coutts ◽  
Franco M Pasutto
Keyword(s):  
Aqueous Solution ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Distilled Water ◽  
Substituted Anilines ◽  
Flame Ionization ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Derivatives Of

Abstract A simple gas-liquid chromatographic (GLC) method has been developed which provides sensitivity and specificity for the analysis of complex mixtures of the commonly occurring herbicide metabolites aniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, and 3-chloro-4-methylaniline. All of these anilines react with acetic anhydride directly in basified aqueous solution. Further reaction of the acetylated anilines with trifluoroacetic anhydride gave diacyl derivatives which were readily resolved by gas chromatography. The structures of the N-acetylated and IV-trifluoroacetylated derivatives of benzylamine (internal standard) and the anilines were confirmed by GLC-mass spectrometry. In distilled water the minimum detectable concentrations of aniline and the substituted anilines, using electron capture GLC, are 0.1 nmole/100 mL and 0.05 nmole/100 mL, respectively. The detection limit for the anilines is 1 nmole/100 ml distilled water, using GLC with flame ionization detection. The technique was applied to the determination of anilines added to urine samples obtained from the general population.

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