Gas Chromatographic Determination of Micro Amounts of Cyanide Residues in Wines, Distilled Liquors, and Other Alcoholic Beverages

1976 ◽  
Vol 59 (6) ◽  
pp. 1390-1395 ◽  
Author(s):  
Brian L Bates ◽  
Donald R Buick
Keyword(s):  
Cyanogen Bromide ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Alcoholic Beverages ◽  
Relative Standard ◽  
Standard Deviations ◽  
Absorber Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of cyanide residues in alcoholic beverages has been developed from procedures previously reported for application to water samples. Quantitatively isolating HCN from alcoholic beverages presented difficulties not encountered with aqueous solutions, particularly in the presence of SO2 in the sample. HCN was liberated from the acidified sample by heating at 70°C, flushed into an NaOH absorber solution, converted to cyanogen bromide (CNBr), extracted into diisopropyl ether, chromatographed on a Porapak Q column, and detected by an electron capture detector. SO2 that is present in most wines interfered with the bromination step and caused low recoveries. This interference was eliminated by initially converting any cyanide present in the sample to the stable mercuric cyanide salt and then purging the acidified sample solution of all SO2. The Hg(CN)2 present was then dissociated by adding KI and the analysis proceeded as previously described. Mean recoveries of 80–97 % were obtained for 2–20 μg cyanide from replicate analyses of spiked samples of distilled liquors free of SO2. The relative standard deviations ranged from 6.1 to 11.1%. Mean recoveries of 65 to 91% were obtained in the same range of cyanide from replicate analyses of spiked wine samples known to contain SO2, with relative standard deviations ranging from 0.8 to 10.2%. The limit of detection was 0.2 μg HCN.

Gas-chromatographic determination of 5-fluorocytosine in human serum.

1976 ◽  
Vol 22 (6) ◽  
pp. 772-776 ◽  
Author(s):  
S A Harding ◽  
G F Johnson ◽  
H M Solomon
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Mean Value ◽  
Normal Serum ◽  
Trimethylsilyl Derivative ◽  
Serum Samples ◽  
Gas Chromatographic Method

Abstract We describe a sensitive and precise gas-chromatographic method, in which cytosine is used as the internal standard, for determination of an antifungal agent, 5-fluorocytosine, in serum. The trimethylsilyl derivative of this drug is well separated from the internal standard and from normal serum constituents. Amphotericin B does not interfere with the determination of 5-fluorocytosine. The lower limit of detection for 5-fluorocytosine is 1 mg/liter when 200 mul of serum is analyzed. Within-run precision (CV), established by analysis of 10 replicates, was 4.5% at a concentration of 19.9 mg/liter. Twenty-five serum samples were analyzed for 5-fluorocytosine by a microbiological assay and by the gas-chromatographic method. Mean value observed with the bioassay was 78.5 mg/liter and with our procedure was 69.4 mg/liter. When values for our assay were regressed against values for the bioassay, slope of the least-squares line was 0.85, intercept was 2.7 mg/liter, and r was 0.93.

Gas Chromatographic Determination of Benalaxyl Residues in Different Crops and Water

1993 ◽  
Vol 76 (3) ◽  
pp. 650-656 ◽  
Author(s):  
Teodoro Crisippi ◽  
Guido Zini ◽  
Riccardo Fabbrini
Keyword(s):  
Gas Chromatography ◽  
Column Chromatography ◽  
Active Ingredient ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Standard Deviations ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described that is suitable for the determination of benalaxyl residues ranging from 10 to 0.1 μg/kg in several crops, must, wine, and water. The compound is extracted with acetone and purified either by partitioning between water and n-hexane or by passing the extract through an Extrelut column with n-hexane. Further purification is achieved by column chromatography on alumina. The active ingredient is finally determined by gas chromatography with nitrogenphosphorus detection. Mean recoveries were ≥95% in the various crops tested and in the 0.01-1.05 mg/kg fortification range. Standard deviations for each crop were ≤6.5%.

scholarly journals Determination of Clopidol Residues in Chicken Tissues by Liquid Chromatography: Part I. Optimization of Analytical Conditions and Comparison with AOAC Gas Chromatography Method

2001 ◽  
Vol 84 (5) ◽  
pp. 1337-1342 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Anion Exchange Column ◽  
Chicken Tissues ◽  
Relative Standard ◽  
Liver And Kidney ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract A simple and specific liquid chromatographic method was developed for determination of clopidol in chicken tissues. Samples were extracted with acetonitrile. The extracts were cleaned up on an alumina column and an anion exchange column. The clopidol was separated on a column (30 cm × 3.9 mm) of μBondapak C18 (10 μm) by using acetonitrile–water (20 + 80, v/v) as mobile phase, and determined quantitatively at 270 nm. Recoveries were 86.0–97.6%, with relative standard deviations of 2.14–9.42% at 0.010–2.0 mg/kg from 4 spiked matrixes of chicken muscle, egg, liver, and kidney. The limit of detection was 0.005 mg/kg. Compared with the modified AOAC gas chromatographic method, the present method is simple and fast to operate. Its results are accurate and reliable, making it favorable for environmental protection and meeting requirements for human safety. Thus, it is suitable for routine analysis of large quantities of samples.

scholarly journals Determination of residual solvents in paclitaxel by headspace gas chromatography

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Khaleel Noorbasha ◽  
Abdul Rahaman Shaik
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Limit Of Detection ◽  
Good Resolution ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Ethyl Amine

Abstract Background A simple and sensitive gas chromatographic method was developed and validated for the simultaneous determination of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine in Paclitaxel. A chromatographic separation was done on DB-624 column, 30 m length × 0.53 mm ID, and film thickness 3 μm, using a flame ionization detector (FID) with gradient column oven temperature program. The injection was carried out in split mode, with a split ratio of 5:1. A mixture of N-methyl-2-pyrrolidinone (contains 1% piperazine) and water in the ratio of 80:20 (v/v) was selected as a diluent to obtain good sensitivity along with the recovery. Results The developed gas chromatographic method offers symmetric peak shape, good resolution of more than 2.0 between the solvent peaks, and the relative standard deviation for replicate injections of all the solvents were found to be not more than 15.0% with reasonable retention time for all the solvents. The limit of detection for methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 304.69 ppm, 497.98 ppm, 498.99 ppm, 504.49 ppm, 61.81 ppm, 30.07 ppm, 505 ppm, 73.05 ppm, and 2.09 ppm, respectively. Limit of quantitation of methanol, ethanol, acetone, isopropyl alcohol, dichloromethane, N-hexane, ethyl acetate, tetrahydrofuran, and N,N-diisopropyl ethyl amine was found to be 89.62 ppm, 146.47 ppm, 146.76 ppm, 148.38 ppm, 18.18 ppm, 8.84 ppm, 148.53 ppm, 21.49 ppm, and 0.62 ppm, respectively. Precision was found to be satisfactory. Linear in the range of LOQ to 150% level for all the solvents, and accuracy along with robustness, is performed, and acceptable results were obtained. Conclusion The proposed method was demonstrated to be simple, sensitive, specific, linear, precise, accurate, and robust, hence can be used to determine the residual organic solvents in Paclitaxel drug substance and drug product.

Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Electron Capture ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Electron Capture Detector ◽  
Reference Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.

Determination of Menthol in Cigarette Tobacco Filler

1967 ◽  
Vol 50 (4) ◽  
pp. 770-773
Author(s):  
Charles L Tucker ◽  
C L Ogg
Keyword(s):  
Chromatographic Method ◽  
Colorimetric Method ◽  
Cigarette Tobacco ◽  
Mean Values ◽  
Accuracy And Precision ◽  
Standard Deviations ◽  
Gas Chromatographic Method

Abstract A gas chromatographic and a colorimetric method for determining menthol in cigarette tobacco filler were studied collaboratively by 15 laboratories. No statistically significant differences were found in the precisions within or between laboratories. There were no significant differences between mean values for the two methods for any of the samples. Trends toward higher mean values for the colorimetric method and lower within-laboratory standard deviations for the gas chromatographic method were noted. Remarks by collaborators suggest that the accuracy and precision of the colorimetric method may be improved, and further studies are recommended.

scholarly journals Gas Chromatographic Determination of Chlorothalonil in Leaves and Roots of Scrophularia and in Soil

1996 ◽  
Vol 79 (2) ◽  
pp. 587-588 ◽  
Author(s):  
Lan Zhao ◽  
De-Fang Fan
Keyword(s):  
Electron Capture ◽  
Chromatographic Method ◽  
Detection Limits ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Florisil Column ◽  
Glass Column ◽  
Leaves And Roots ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for determination of chlorothalonil residues in leaves and roots of Scrophularia and in soil. Samples were extracted with acetone and cleaned up on a Florisil column. Chlorothalonil residues are chromatographed directly on a glass column of 1.5% OV-17 and 2% QF-1 coated on 80-100 mesh Chromosorb W (HP) support and measured with a 63Ni electron capture detector. Detection limits are 0.001 ppm for leaf, 0.005 ppm for root, and 0.001 ppm for soil.

Capillary Column Gas Chromatographic Determination of Trace Residues of the Herbicide Chlorsulfuron in Agricultural Runoff Water

1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Chromatographic Determination ◽  
Agricultural Runoff ◽  
Runoff Water ◽  
Florisil Column ◽  
Gas Chromatographic Method

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.

Gas Chromatographic Determination of Histapyrrodine Hydrochloride in Pharmaceutical Preparations

1986 ◽  
Vol 69 (4) ◽  
pp. 612-613
Author(s):  
Ramesh T Sane ◽  
Vipul J Doshi ◽  
Sanjay K Joshi ◽  
Vijay K Shastri ◽  
Dhananjay S Sapre ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Chromatographic Determination ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Label Claim ◽  
Gas Chromatographic Method

Abstract A simple gas chromatographic method is described for the determination of histapyrrodine HC1 in marketed formulations. Chlorpheniramine maleate is used as the internal standard. The amount of histapyrrodine HC1 found by the proposed method averaged 19.91 mg/tablet, compared with the label claim of 20 mg/tablet. The method was statistically evaluated for accuracy and precision.

scholarly journals Gas Chromatographic Determination of Butylated Hydroxyanisole (BHA) and Butylated Hydroxytoluene (BHT) in Products Containing Capsaicinoids

1996 ◽  
Vol 79 (6) ◽  
pp. 1459-1462
Author(s):  
Bernard DeWitt ◽  
Gunnar Finne
Keyword(s):  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Butylated Hydroxytoluene ◽  
Butylated Hydroxyanisole ◽  
Liquid Chromatographic Method ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract Because of interference by coeluting capsaicinoids, the commonly used liquid chromatographic method for determining butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in pepperoni and spice blends is not reliable. A gas chromatographic method is described that cleanly separates these antioxidants from interfering substances. Average recoveries of BHA and BHT from oleoresin spiked at 5 concentrations were 97.6 and 104.3%, respectively. From pepperoni spiked at 4 levels, average recoveries were 79.1 and 87.9%, respectively. The repeatability of the method when applied to 5 replicates of pepperoni toppings was 36.4 ± 1.1 ppm for BHA and 32.2 ± 0.8 ppm for BHT.

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