Gas Chromatographic Determination of Total Active Ingredient Content of Karathane Technical and Karathane WD. I. Development of the Method

1970 ◽  
Vol 53 (5) ◽  
pp. 887-895
Author(s):  
C P Kurtz ◽  
H Baum ◽  
C Swithenbank
Keyword(s):  
Active Ingredient ◽  
Silicone Oil ◽  
Internal Standard ◽  
Direct Determination ◽  
Chromatographic Determination ◽  
Working Standard ◽  
Column Temperature ◽  
Glass Column ◽  
In Series

Abstract A new GLC method for the direct determination of the active ingredient in Karathane Technical and Karathane WD is presented. The internal standard (4,6-dinitro-o-cresol) in nitrobenzene solution is added to the sample, or the extract residue in the case of Karathane WD, and the solution is chromatographed on a flame ionization instrument, using an 8’ glass column packed with 3% QF-1 silicone oil on 60–80 mesh Gas Chrom Q. Column temperature is programmed from 100 to 230°C. A working standard of known composition is run in the same manner in series with the sample. The precision of a single determination of the total 2,4- and 2,6-dinitrooctylphenyl crotonate isomers (about 74%) in Karathane Technical and the total dinitrooctylphenols and mononitrooctylphenols (about 6%) is s = 0.5% absolute. Data on the analysis of a limited number of Karathane WD samples show good agreement for the total active ingredient.

Liquid Chromatographic Determination of Acids and Sugars in Homolactic Cucumber Fermentations

1989 ◽  
Vol 72 (1) ◽  
pp. 52-55
Author(s):  
Maria Jesus Lázaro ◽  
Elvira Carbonell ◽  
Maria Concepcion Aristoy ◽  
Jose SafÓn ◽  
Miguel Rodrigo
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
High Yield ◽  
Column Temperature ◽  
In Series ◽  
Liquid Chromatographic Determination ◽  
Standard Values ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A rapid, high yield, and quantitative method for determination of sugars (glucose and fructose) and acids (malic, lactic, acetic, and citric) in fresh and fermented cucumber juices is described; the procedure solves the fructose and malic acid coelution problem. Samples are prepared by passing the juice directly through a disposable C18 cartridge. Compounds are separated by liquid chromatography on an Aminex HPX-87H chromatographic column, with 0.013N H2S04 as mobile phase in the isocratic mode at 0.6 mL/min flow rate and 60°C column temperature. Compounds are then detected and quantitated by using ultraviolet and refractive index detectors connected in series, and comparing with succinic acid as internal standard. Values for both fresh and fermented cucumber juices were in good agreement with literature data.

Capillary Gas Chromatographic Determination Of Cypermethrin In Formulations: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 592-595
Author(s):  
Peter D Bland
Keyword(s):  
Active Ingredient ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Fused Silica ◽  
Flame Ionization ◽  
Wettable Powder ◽  
Peak Areas ◽  
Liquid Concentrate

Abstract A method is described for the determination of cypermethrin, 3-(2,2- dichloroethenyl)-2,2-dimethyl-cyclopropanecarboxylate cyano-(3- phenoxyphenyl)methyl ester, in technical and formulated material by capillary gas chromatography (CGC). Samples of technical or formulated material are dissolved in CH2Cl2 containing dicyclohexyl phthalate as internal standard. The solution is injected into a gas chromatograph fitted with a flame ionization detector and capillary column of 25 m x 0.32 mm fused silica with a thick film OV-1 phase at 240°C. Injection is made into a heated injection port fitted with an antidiscrimination device in a split mode. Peak areas obtained at retention times of the internal standard and active ingredient are measured with an integrator. The quantity of cypermethrin is determined by comparing the internal standard and active ingredient peak areas with those obtained from a calibration solution containing known amounts of internal standard and pure active ingredient. Five samples were chosen for collaborative study: technical cypermethrin, 70% liquid concentrate, 3 lb/US gal. emulsifiable, 3 ib/US gal. oil concentrate, and 40% wettable powder. Twelve collaborators carried out replicate determinations on each sample on separate days. Coefficients of variation between laboratories (CVX) were 2.13 for the technical, 2.94 for the emulsifiable concentrate, 3.51 for the liquid concentrate, 2.66 for the wettable powder, and 2.29 for the oil concentrate. The method was adopted official first action.

Gas-Solid Chromatographic Determination of Oxygen, Nitrogen, Carbon Dioxide, Ethylene, and Nitrous Oxide at Ambient Temperature

1973 ◽  
Vol 56 (1) ◽  
pp. 119-123
Author(s):  
Martin J Finkelson
Keyword(s):  
Carbon Dioxide ◽  
Nitrous Oxide ◽  
Ambient Temperature ◽  
Molecular Sieve ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Digital Integrator ◽  
In Series ◽  
Peak Areas

Abstract A gas-solid chromatographic method is described for the separation and determination of 5 medicinal gases at ambient temperature, using 2 gas chromatographic columns, Porapak Q and Molecular Sieve 13X, operated in series with a 6-port thermal conductivity detector and I recorder. An electronic digital integrator is used for calculating peak areas. Data on retention time, linearity, reproducibility of injection, and comparison with absorption methods are presented. Analytical results for oxygen, nitrogen, carbon dioxide, ethylene, and nitrous oxide are attainable within 1.0% without the use of an internal standard.

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 Chromatographic Determination of Metolachlor in Pesticide Formulations: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 570-572
Author(s):  
Thomas G Gale ◽  
Arthur H Hofberg
Keyword(s):  
Active Ingredient ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Matched Pair ◽  
Emulsifiable Concentrate ◽  
Flame Ionization ◽  
Pesticide Formulations ◽  
Better Than

Abstract A gas chromatographic (GC) procedure for the determination of metolachlor in emulsifiable concentrate formulations containing about 76% active ingredient was collaboratively studied using the matched pair scheme. Metolachlor was extracted from the formulation with acetone containing dipentyl phthalate as the internal standard, chromatographed on OV-101, and detected by flame ionization. Determinations on the 4 samples by 21 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 0.5%. Reproducibility was better than 1% for the formulation. The method has been adopted official first action.

Simultaneous liquid-chromatographic determination of 12 common sedatives and hypnotics in serum.

1978 ◽  
Vol 24 (4) ◽  
pp. 657-662 ◽  
Author(s):  
P M Kabra ◽  
H Y Koo ◽  
L J Marton
Keyword(s):  
Serum Proteins ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Acetonitrile Solution ◽  
Column Temperature ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We present a method for simultaneously determining 12 hypnotics and sedatives (primidone, methyprylon, phenobarbital, butabarbital, butalbital, ethchlorvynol, pentobarbital, amobarbital, phenytoin, glutethimide, secobarbital and methaqualone) in 200 microliter of serum. Serum proteins are precipitated with an acetonitrile solution containing 5-(4-methylphenyl)-5-phenylhydantoin, the internal standard. The drugs are eluted from a reversed-phase column with a mobile phase consisting of an acetonitrile/phosphate buffer, at a flow rate of 3.0 ml/min. The eluted drugs are detected by their absorption at 195 nm; their quantities are estimated from their peak heights. Each analysis requires no longer than 30 min at the optimum column temperature of 50 degrees C. The lower limit of detection for all of these drugs is less than 10 ng/sample for drug standard. A sensitivity of 1.0 mg/liter of serum is attained routinely for each of the drugs. Analytical recoveries for the 12 drugs varied from 94 to 112%, with good day-to-day precision (CV between 3.8 and 10.4%). Of more than 35 drugs tested for possible interference, only ethotoin interferes with the analysis of phenobarbital.

Gas Chromatographic Determination of Propionic Acid in Bread and Cake

1981 ◽  
Vol 64 (2) ◽  
pp. 280-281
Author(s):  
Kenji Isshiki ◽  
Shusaku Tsumura ◽  
Tadao Watanabe
Keyword(s):  
Formic Acid ◽  
Propionic Acid ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Accurate Method ◽  
Isobutyric Acid ◽  
Bakery Products ◽  
System A ◽  
Glass Column

Abstract A simple and accurate method is presented for gasliquid chromatographic (GLC) determination of propionic acid in bakery products. Propionic acid is extracted with a mixture of dichloromethane and formic acid to which isobutyric acid has been added as an internal standard. The extract is injected directly into the GLC system. A glass column packed with 5% SP-1000 is used. The simplicity and convenience of the method make it suitable for routine determination.

Gas-Liquid Chromatographic Determination of Adipate Content of Acetylated Di-starch Adipate

1982 ◽  
Vol 65 (2) ◽  
pp. 238-240
Author(s):  
Gordon A Mitchell ◽  
Michel J Vanderbist ◽  
Florent F Meert
Keyword(s):  
Ethyl Acetate ◽  
Adipic Acid ◽  
Silicone Oil ◽  
Internal Standard ◽  
Active Phase ◽  
Chromatographic Determination ◽  
Silyl Derivative ◽  
Alkaline Conditions ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method is described for rapid, quantitative determination of adipate content of acetylated di-starch adipate. The adipate group is very labile and, under mild alkaline conditions at ambient temperature, is easily hydrolyzed from the starch. Free adipic acid is formed by acidification of the solution with HC1, and then extracted with ethyl acetate. Ethyl acetate is removed under vacuum distillation, and a silyl derivative of the adipic acid is formed. Glutaric acid internal standard is introduced into the original starch sample before hydrolysis. An aliquot of the silylated solution is injected into a gas chromatograph fitted with a column having silicone oil as the active phase. A flame ionization detector is also incorporated. Results correlate well with the amount of adipylating reagent used. No adipic acid is detectable when a hydrolyzed, extracted sample of acetylated di-starch adipate is subjected to a second extraction. Recovery levels of adipic acid, from starches fortified with 100-500 ppm, are in the range of 97-102.5.%

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 Chromatographic Determination of Chlordimeform in Pesticide Formulations: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 589-592
Author(s):  
Thomas G Gale ◽  
Arthur H Hofberg
Keyword(s):  
Active Ingredient ◽  
Methylene Chloride ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Matched Pair ◽  
Flame Ionization ◽  
Pesticide Formulations ◽  
Better Than

Abstract Agaschromatographic (GC) procedure for the determination of chlordimeform in emulsiflable concentrate formulations containing about 46% active ingredient was collaboratively studied using the matched pair scheme. Chlordimeform was extracted from the formulation with methylene chloride containing diethyl terephthalate as the internal standard, chromatographed on CBWX-20M, and detected by flame ionization. Determinations on the 4 samples by 20 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 1%. Reproducibility was 1.2% for the formulation. The method has been adopted official first action.

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