GLC Determination of Methanol in Liquids: Collaborative Study

1971 ◽  
Vol 54 (3) ◽  
pp. 558-559
Author(s):  
Donald L Andersen

Abstract A rapid, specific method for methanol in aqueous and nonaqueous liquids has been developed and studied collaboratively. The method involves sample dilution with dioxane to approximately 0.4% methanol and injection into a gas chromatograph fitted with a Porapak R column and a flame ionization detector. A collaborative study, with 7 collaborators each reporting on 6 test portions, showed coefficients of variation of 2.7, 2.1, 2.3, 4.2, 1.8, and 3.5. The method has been adopted as official first action.

1969 ◽  
Vol 52 (3) ◽  
pp. 435-438
Author(s):  
Albert J Gehrt

Abstract A GLC method (flame ionization detector) for ronnel in cattle feeds at levels of 0.038, 0.041, and 0.055% was studied by 11 collaborators. The method involves extraction of ronnel by shaking with acetone followed by direct chromatographic measurement. The method is simple and rapid (no cleanup required), measures true ronnel, and is free from interferences present in the UV methods previously studied. Agreement between laboratories was satisfactory; coefficients of variation were 11.0, 12.0, and 7.2%. Ronnel recoveries were 81.1, 93.5, and 98.0%. Low recovery from the first sample may be due to ronnel hydrolysis or binding during storage (sample was 8 months old). The Associate Keferee recommends that the method be adopted as official first action.


1974 ◽  
Vol 20 (11) ◽  
pp. 1460-1462 ◽  
Author(s):  
Naresh C Jain ◽  
Thomas C Sneath ◽  
Robert D Budd

Abstract A simple, rapid procedure is described for measuring amphetamine and methamphetamine in urine by gas chromatography, with use of a flame ionization detector. This method is sensitive to subtherapeutic concentrations (0.1 µg/ml or less), and is especially useful in clinical situations where an accurate and quantitative result is needed in less than 30 min. With the method, amphetamine and methamphetamine can be determined as the free bases on a 10% Apiezon L-10% KOH column and as their trifluoroacetamide derivatives on a 3% OV-17 column. This dual analysis eliminates false positives and any interfering substances that may be present in the urine, and is thus a specific method for the two drugs.


1973 ◽  
Vol 22 (2) ◽  
pp. 95-101
Author(s):  
Shoichiro WATANABE ◽  
Satoshi NAKASATO ◽  
Hideo KUWAYAMA ◽  
Yukihiro SASAMOTO ◽  
Shinsaku SHIRAISHI ◽  
...  

1978 ◽  
Vol 61 (1) ◽  
pp. 164-166
Author(s):  
Fred A Moseley ◽  
Joel S Salinsky ◽  
Robert W Woods

Abstract A rapid and simple method of analysis has been developed for sorbitol in cooked sausage products. Sorbitol is extracted from cooked sausage products with water, an aliquot of the extract is freeze-dried, and the trimethylsilyl (TMS) derivative of sorbitol is formed. An aliquot of the TMS-sorbitol is injected into a gas chromatograph and measured by a flame ionization detector. Analysis of fortified samples shows that the recovery compares well with known amounts of sorbitol added.


1972 ◽  
Vol 55 (6) ◽  
pp. 1331-1335 ◽  
Author(s):  
A A Carlstrom

Abstract The GLC method described is specific for measuring 4 components of Phosphamidon Insecticide—deschlorophosphamidon, α-phosphamidon, β-phosphamidon, and γ-chlorophosphamidon. The sample is extracted with acetone, an internal standard (dicyclohexyl phthalate) is added, and the solution is diluted to volume and injected into a gas chromatograph equipped with a flame ionization detector. Although the GLC peak areas for phosphamidon are not linear over a wide range of concentration, good results are obtained when sample and standard concentrations are matched to within 10%. A 1.21% coefficient of variation was found for 19 repetitive injections.


1974 ◽  
Vol 57 (1) ◽  
pp. 53-59
Author(s):  
James E Barney

Abstract Eptam, Ordram, Ro-Neet, Sutan, Tillam, and Vernam thiocarbamate herbicides are determined in emulsifiable and granular formulations by gas chromatography on an OV-1, SE-30, or OV-17 column with a flame ionization detector. Another thiocarbamate is used as an internal standard. The method was tested collaboratively by 19 laboratories, 18 of which tested the method on all 6 thiocarbamates. The coefficient of variation for 12 formulations was 3.10%. A significant amount of systematic error was detected, particularly in the analysis of emulsifiable formulations. The method has been adopted as official first action, and it is recommended that additional studies be conducted.


2021 ◽  
Vol 17 ◽  
Author(s):  
Fatang Yang ◽  
Xiaoyun Duan ◽  
Zhen Wang ◽  
Yuming Dong

Aims: To establish a rapid and simultaneous determination of multiple effective ingredients in anti-cold drugs. Background: Anti-cold drugs are stock medicines at home, and most anti-cold formulations are compound preparations. Although the active ingredients of compound preparations have significant effects on the treatment of colds, the excessive dosage or long-term use can produce a series of adverse reactions including dependence, liver and kidney function damage, digestive system reaction, blood system damage. Now, there are many mature methods for analyzing the active ingredients of anti-cold drugs. However, these methods may have shortcomings such as a long analysis time or a small number of analysis components. Objective: Establish a gas chromatography-flame ionization detector method for the simultaneous determination of six active ingredients including acetaminophen, dextromethorphan hydrobromide, pseudoephedrine hydrochloride, chlorpheniramine maleate, diphenhydramine hydrochloride, and caffeine in anti-cold drugs. Method: After the standard was accurately weighed, dissolved in ethanol, filtered by 0.22 μm membrane and ultrasonically degassed, the gas chromatograph was used for detection. After the actual sample was removed from the coating, ground and crushed, accurately weighed, dissolved in ethanol, filtered by 0.22 μm membrane and ultrasonically degassed, the gas chromatograph was used for detection. Result: The six components can be completely separated within 7.0min. This method has good sensitivity, precision, accuracy and recovery rate. Under the optimum testing conditions, the limit of detection was 0.360-2.50μg/mL, the limit of quantification was 1.20-8.30μg/mL. The calibration curves showed good linearity (R2≥0.9932) over the investigated concentration range between 1.20 and 400μg/mL. The recoveries were 89.2% to 109.2%. The RSD of intra-day precision was less than 1.0%. The RSD of inter-day precision was less than 3.2%. The established method was used to determine the ingredients of three anti-cold drugs on the market, and the results showed that the method can accurately determine the ingredients. Conclusion: The method can quickly and simultaneously determine multiple active ingredients in anti-cold medicines. Compared with the published methods in literatures, the proposed method has the advantages of fast, the number of analysis componentswide application range, convenience, low cost, etc. It provides a reference method for quality control of active ingredients of anti-cold drugs.


1971 ◽  
Vol 54 (1) ◽  
pp. 125-127
Author(s):  
Larry G Hambleton

Abstract A gas chromatographic method has been developed that is rapid and specific for trifluralin in formulations. The sample is extracted with acetone, an internal standard is added, and the solution is diluted to volume and injected into a gas chromatograph equipped with a flame ionization detector. Three typical trifluralin formulations were analyzed by both the gas chromatographic method and an ultraviolet method. The gas chromatographic method gave an average recovery of 101.2%.


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