scholarly journals Sampling and Analytical Method for Alpha-Dicarbonyl Flavoring Compounds via Derivatization witho-Phenylenediamine and Analysis Using GC-NPD

Scientifica ◽  
2016 ◽  
Vol 2016 ◽  
pp. 1-10
Author(s):  
Stephanie M. Pendergrass ◽  
Jeffrey A. Cooper

A novel methodology is described for the sampling and analysis of diacetyl, 2,3-pentanedione, 2,3-hexanedione, and 2,3-heptanedione. These analytes were collected ono-phenylenediamine-treated silica gel tubes and quantitatively recovered as the corresponding quinoxaline derivatives. After derivatization, the sorbent was desorbed in 3 mL of ethanol solvent and analyzed using gas chromatography/nitrogen-phosphorous detection (GC/NPD). The limits of detection (LOD) achieved for each analyte were determined to be in the range of 5–10 nanograms/sample. Evaluation of the on-tube derivatization procedure indicated that it is unaffected by humidities ranging from 20% to 80% and that the derivatization procedure was quantitative for analyte concentrations ranging from 0.1 μg to approximately 500 μg per sample. Storage stability studies indicated that the derivatives were stable for 30 days when stored at both ambient and refrigerated temperatures. Additional studies showed that the quinoxaline derivatives were quantitatively recovered when sampling up to a total volume of 72 L at a sampling rate of 50 cc/min. This method will be important to evaluate and monitor worker exposures in the food and flavoring industry. Samples can be collected over an 8-hour shift with up to 288 L total volume collected regardless of time, sampling rate, and/or the effects of humidity.

2014 ◽  
Vol 687-691 ◽  
pp. 4515-4519
Author(s):  
Jian Chun Zhao

In this paper, yam functional food technology and storage stability were studied, the results indicate that storage time and temperature on the results significantly higher than room temperature sample storage, cryogenic sample index changes significantly, the moisture content of the sample affect the sensory scores larger.


1994 ◽  
Vol 77 (4) ◽  
pp. 942-947 ◽  
Author(s):  
Yichun Xu ◽  
Chester J Mirocha

Abstract An analytical method for detection of wortmannin in corn kernels was developed based on liquid chromatography (LC) and gas chromatography (GC). The sample was extracted with ethyl acetate, subjected to cleanup procedures on Sep–Pak silica gel column, and eluted with dichloromethane–chloroform (1+1). Analysis was made either by LC or GC. The limit of detection was 2.5 by LC and 25 ng/g by GC. The recovery from corn by LC at 2.5, 5.0, 10, 25, 50, 100, 250, 500, and 1000 ng/g was 89 (11.5 sd), 72 (2.6), 69 (7.4), 90 (7.5), 78 (9.3), 72 (6.1), 84 (17.5), 82 (11.5), and 76 (12.9), respectively. Recovery measured by GC at 25, 50, 100, 250, 500, and 1000 ng/g was 78 (12.5), 72 (14.0), 78 (3.8), 69 (2.6), 74 (16.9) and 81 (8.3)%, respectively. The average recovery was 79% by LC and 75% by GC.


2011 ◽  
Vol 46 (4) ◽  
pp. 341-349 ◽  
Author(s):  
Patrizia Stefanelli ◽  
Danilo Attard Barbini ◽  
Silvana Girolimetti ◽  
Angela Santilio ◽  
Roberto Dommarco

Author(s):  
Mizutani G ◽  
◽  
Bustillos O ◽  

Beans are part of the basic diet alimentation for Brazilian population, as they gather proteins, carbohydrates, vitamins, mineral salts, fibers, amino acids and essential nutrients such as iron and calcium, being a complete food that can be compared with the amount of protein that the meat has. Considering the beans world production, in development countries represent almost 50%, being that Myanmar, India and Brazil the top three position. The use of pesticides is widely spread in these countries to reduce agricultural losses due to pests that interfere with grain production. Therefore the risk that could be generated from foods pesticides residues makes their analyses of quantification mandatory. The purpose of this work was to develop an analytical method to quantitatively characterize fungicides pesticides residues, flutriafol, procymidone and tebuconazole that were used to angular spot control, anthracnose, rust and alternaria spot, white mold fungi, present in beans, by means of gas chromatography coupled with a triple quadrupole mass spectrometer. Samples of beans, Phaseolus vulgaris L, types white, black, string and Vigna angularis, type adzuki, had been bought in grains store and supermarkets at metropolitan São Paulo city. The validation of analytical method was explored for sensitivity, selectivity, precision. The extraction procedure was performed in two different forms, QuEChERS, and solid-liquid extraction with low temperature. Through this methodology, reached below the maximum limit allowed by Brazilian law 0.5mgkg-1 for procymidone and 0.1mgkg-1 for flutriafol and tebuconazole. Several samples of four types of beans were tested and all of them had procymidone identified and 7% of samples higher than the law limit.


Author(s):  
L.N. Schitov ◽  
Y.A. Dzhurko ◽  
A.V. Volkov ◽  
E.V. Baskakov ◽  
I.A. Kabanova ◽  
...  

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