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G W Diachenko

Publications and source records attributed to G W Diachenko.

24 records · Page 2Linked to original sources

Measurement of bromate in bottled water by high-performance liquid chromatography with post-column flow reactor detection.

The objective of this work was to develop a reliable, rugged high-performance liquid chromatographic (HPLC) method for determination of trace levels of bromate (< 10 micrograms/l) in bottled water. HPLC separation was achieved by ion interaction chromatography using a C-18 reversed-phase column and a mobile phase consisting of methanol/water (20:80, v/v) with tetrabutylammonium acetate as the ion interaction reagent. A post-column reaction based on oxidation of o-dianisidine in acidic solution to a product detected at 500 nm provided selective measurement of the oxidants. The limit of detection and the limit of quantitation were 1 and 3 micrograms/l, respectively. Iodate, chlorite, and nitrite were chromatographically separated from bromate and measured by monitoring the post-column reaction. Chloride and chlorate at levels that might be found in bottled water did not interfere with the determination of bromate. Bromate was detected in bottled waters at concentrations up to 40 micrograms/l.

Bromates↗

Ethyl carbamate levels in selected fermented foods and beverages.

Ethyl carbamate (EC), also known as urethane, is an animal carcinogen and a by-product of fermentation. Because EC has been found in distilled spirits and wines, a variety of fermented foods and beverages were analyzed to assess its occurrence in other products. Previously described methods using a gas chromatograph-thermal energy analyzer with a nitrogen converter were modified for each matrix and gave recoveries of greater than 80%, with a limit of detection in the 1-2 micrograms/kg (ppb) range. A total of 152 test samples were analyzed; EC levels ranged from none found to 3 ppb in 15 cheeses, 6 teas, 12 yogurts, and 8 ciders; from none found to 13 ppb in 30 breads and 69 malt beverages; and from none found to 84 ppb in 12 soy sauces. Gas chromatography/mass spectrometry/mass spectrometry was used to confirm EC identity and to quantitate EC in selected food extracts.

Alcoholic Beverages↗

Liquid chromatographic determination of sulfite in grapes and selected grape products.

A liquid chromatographic (LC) method is described for the determination of sulfite in grapes and certain grape products. Sulfite is extracted from grapes with aqueous formaldehyde solution buffered at pH 5; free sulfite is converted to hydroxymethylsulfonate (HMS), which is extremely stable at pH 3-7. Subsequent heating to 80 degrees C for 30 min converts reversibly bound forms of sulfite to HMS. The extract is then analyzed by reverse-phase ion-pairing liquid chromatography, using a C18 column and a mobile phase of aqueous 0.005 M tetrabutylammonium ion in 0.05 M acetate, pH 4.7, and a flow rate of 1 mL/min. Aqueous KOH is added to the eluate to convert HMS to free sulfite, which is then treated with 5,5'-dithiobis[2-nitrobenzoic acid]. This reaction produces the 3-carboxy-4-nitrothiophenolate anion, which is determined by measurement of electronic absorption at 450 nm. For grapes spiked with HMS at 5-20 ppm (as SO2), recoveries ranged from 92 to 112%, with a coefficient of variation of 4.6%. The method was also used to determine sulfite in various grape products. Results were comparable to those obtained by the AOAC official Monier-Williams method.

Chromatography, Liquid↗

Survey of trihalomethanes and other volatile chemical contaminants in processed foods by purge-and-trap capillary gas chromatography with mass selective detection.

A limited number of soft drinks, juices, beers, and waters from processed vegetables were analyzed for trihalomethanes (THMs), benzene, and toluene by a modified Environmental Protection Agency (EPA) Method 524.2. The THMs, which include chloroform, bromodichloromethane, dibromochloromethane, and bromoform, are reaction by-products of water disinfection by chlorination. EPA Method 524.2 is a purge-and-trap capillary gas chromatographic method based on mass spectrometric detection which identifies and simultaneously measures purgeable volatile organic compounds in drinking water. Chloroform was present at concentrations ranging from none detected to 94 ng/g in the 44 foods analyzed. Bromoform was not found in any of the products at a detection limit of 0.1 ng/g. Residue levels of the other THMs ranged from none detected to highs of 12 and 2 ng/g for bromodichloromethane and dibromochloromethane, respectively. Benzene residues were typically < 5 ng/g, except for 7 and 9 ng/g in 2 foods. Toluene residues were typically < or = 3 ng/g except for 23, 29, and 75 ng/g in 3 canned foods.

Benzene↗

Determination of ethyl carbamate in alcoholic beverages and soy sauce by gas chromatography with mass selective detection: collaborative study.

A method using gas chromatography with mass selective detection for the determination of ethyl carbamate (EC; also known as urethane) in alcoholic beverages and soy sauce was collaboratively studied by 17 laboratories including authors' laboratories. The method uses prepacked columns for extraction of liquids with methylene chloride, and n-propyl carbamate as the internal standard. A practice sample and 6 samples of distilled spirits, fortified wines, table wines, and soy sauces were analyzed by each collaborator. Each matrix included blind duplicates of incurred and fortified EC at 3 levels. Distilled spirits contained 50-330 ng EC/g (ppb), fortified wine 40-160 ppb, table wine 10-50 ppb, and soy sauce 15-70 ppb. The ranges of the repeatability relative standard deviations, excluding outliers, were 4.03-6.63% for distilled spirits, 4.01-5.05% for fortified wine, 3.94-6.73% for table wine, and 4.70-8.49% for soy sauce. The ranges of the reproducibility relative standard deviations, excluding outliers, were 8.53-9.49% for distilled spirits, 6.84-12.02% for fortified wine, 8.86-18.47% for table wine, and 13.87-27.37% for soy sauce. Recoveries of added EC ranged from 87 to 93%. Recoveries relative to reference values, labeled as the internal standard, obtained by using gas chromatography/tandem mass spectrometry with a triple quadrupole mass spectrometer ranged from 89 to 100%.

Alcoholic Beverages↗

Survey of benzene in foods by using headspace concentration techniques and capillary gas chromatography.

Recently, the combination of sodium or potassium benzoate with ascorbic acid was shown to produce low levels (ng/g) of benzene in fruit-flavored soft drinks. The presence of benzene also was reported in butter, eggs, meat, and certain fruits; levels of these findings ranged from 0.5 ng/g in butter to 500-1900 ng/g in eggs. Because benzoates are widely used as food preservatives, a limited survey of other foods containing added benzoate salts was conducted to investigate the potential for benzene formation. Selected foods that did not contain added benzoates but were previously reported to contain benzene were analyzed for comparison. More than 50 foods were analyzed by purge-and-trap or static headspace concentration and capillary gas chromatography. Benzene was quantitated by using the method of standard additions, and its identity was confirmed by mass selective detection. Results of this limited survey show that foods without added benzoates (including eggs) contained benzene at levels equal to or less than 2 ng/g. Slightly higher levels were present in some foods and beverages containing both ascorbic acid and sodium benzoate.

Benzene↗