An efficient method for measuring dissolved VOSCs in wastewater using GC-SCD with static headspace technique

Volatile organic sulfur compounds (VOSCs) are important sources of unpleasant odor in wastewater systems. However, the study of VOSCs is usually hindered by their complicated measurement method and highly reactive nature. In this work, a static headspace method utilising gas chromatography (GC) with a sulfur chemiluminescence detector (SCD) was developed to quantitatively analyze VOSCs in wastewater matrices. The method has low detection limits and requires no pre-concentration treatment. Three typical VOSCs, namely methanethiol (MT), dimethyl sulfide (DMS) and dimethyl disulfide (DMDS), were chosen as examples for this study. The calibration curves of all three compounds covering a wide range from 0.5 ppb to 500 ppb showed good linearity (R-2 > 0.999). The method detection limits (MDL) were 0.08, 0.12 and 0.21 ppb for MT, DMS and DMDS, respectively. The reproducibility (relative standard deviation) was approximately 2%. The recovery ratio of MT, DMS and DMDS in spiked wastewater samples were 83 +/- 4%, 103 +/- 4% and 102 +/- 3%, respectively. Sample preservation tests showed that VOSCs in wastewater samples could be preserved in vials without headspace under acidified conditions (pH similar to 1.1) for at least 24 h without significant changes

Comparison of aroma volatiles in commercial Merlot and Cabernet Sauvignon wines using gas chromatography - olfactometry and gas chromatography - mass spectrometry

Seventy-four aroma active compounds were observed in Merlot and Cabernet Sauvignon wines produced in California and Australia. Volatiles were sampled using solid phase microextraction and analyzed using time-intensity gas chromatography-olfactometry and gas chromatography-mass spectrometry (GC-MS). The most intense odorants were 3-methyl-1-butanol, 3-hydroxy-2-butanone, octanal, ethyl hexanoate, ethyl 2-methylbutanoate, beta-damascenone, 2-methoxyphenol, 4-ethenyl-2-methoxy-phenol, ethyl 3-methylbutanoate, acetic acid, and 2-phenylethanol. Aroma compounds were classified according to their aroma descriptor similarity and summed into nine distinct categories consisting of fruity, sulfury, caramel/cooked, spicy/peppery, floral, earthy, pungent/chemical, woody, and green/vegetative/fatty. Both Merlot and Cabernet Sauvignon wines were characterized by high fruity, caramel, green, and earthy aroma totals. Although there were distinct quantitative differences between Merlot and Cabernet wines, the relative aroma category profiles of the four wines were similar. Of the 66 volatiles identified by GC-MS, 28 were esters and 19 were minor alcohols. Between 81 and 88% of the total MS total ion chromatogram peak areas from each wine type were produced from only eight compounds: ethanol, ethyl octanoate, ethyl decanoate, ethyl acetate, 3-methyl-1-butanol, ethyl hexanoate, diethyl succinate, and 2-phenylethanol. Merlot wines from both Australia and California contained 4-5 times more ethyl octanoate than Cabernet Sauvignon wines from the same sources

Identification of muscadine wine sulfur volatiles: Pectinase versus skin-contact maceration

Muscadine grapes (Vitis rotundifolia) are widely grown in the southern United States, as the more common Vitis vinifera cannot be cultivated due to Pierce's disease. There is interest to determine if certain cultivars can be used for good-quality wine production. This study compared the effect of pectolytic enzyme pretreatment with conventional skin-contact fermentation on Muscadine (Noble, Vitis rotundifolia) wine major volatiles, aroma active volatiles, and volatile sulfur compounds (VSCs). Volatile composition, aroma activity, and VSCs in the initial juice and wine samples after 3 years were determined by gas chromatography in combination with mass spectrometry (GC-MS), olfactory detection (GC-O), and pulsed flame photometric detection (GC-PFPD). Forty-three nonethanol MS volatiles were common to all samples. Total ion chromatogram (TIC) MS peak area increased 91% in the skin-contact wines from the initial juice but only 24% in the enzyme-treated wine. Thirty-one VSCs were detected. Twenty-four sulfur volatiles were identified by matching their retention characteristics on polar and nonpolar columns with those of standards or MS spectrum matches. Six of these (sulfur dioxide, 1-propanethiol, 3-mercapto-2-pentanone, 3-mercapto-2-butanone, 2,8-epithio-cis-p-menthane, and 1-p-menthene-8-thiol) were reported for the first time in muscadine wine. Five additional VSCs were tentatively identified by matching standardized retention values with literature values, and two remain unidentified. Total sulfur peak areas increased 400% in the skin-contact wine and 560% in the enzyme-treated wine compared to the initial juice. There were 42 aroma-active volatiles in the initial juice, 48 in the skin-contact wine, and 66 in the enzyme-treated wine. Eleven aroma-active volatiles in the skin-contact wine and 16 aroma volatiles in the enzyme-treated wine appear to be due to sulfur volatiles. Pectolytic enzyme-treated wines contained less total volatiles but more sulfur and aroma-active volatiles than the traditional skin-contact wine.University of Florida, IFAS, CREC, Lake Alfred, F

Novel off-flavors produced from the thermophillic bacteria, Alicyclobacillus acidoterrestris, in pineapple juice

International audienc

Analysis of grapefruit sulphur volatiles using SPME and pulsed flame photometric detection

Sulphur volatiles are major factors in the perceived aroma of grapefruit juice, GFJ. The objective of this study was to develop a procedure to concentrate, separate, identify and quantify the major volatile sulphur compounds, VSC's, in grapefruit juices. SPME parameters such as headspace atmosphere, fibre coating, extraction time and temperature were evaluated. High resolution capillary CC using ZB-5, DB-Wax and PLOT columns coupled with pulsed flame photometric detection, PFPD, were employed for separation and detection. Thirteen sulphur volatiles were identified including; hydrogen sulphide, sulphur dioxide, methanethiol, dimethyl sulphide, carbon disulphide, dimethyl disulphide, 2-methyl thiophene, 3-methyl thiophene, methional, dimethyl trisulphide, 3-mercaptohexylacetate, 2,8-epithio-cis-p-menthane and 1-p-menthene-8-thiol. Five additional VSC's were tentatively identified. Canned reconstituted GFJ had more total sulphur volatiles and a greater number than fresh GFJ. Hydrogen sulphide comprised over 80% of total sulphur volatiles in fresh GFJ but only 5% in canned GFJ.University of Florida Alumni Fellowship Foundatio

Novel off-flavors produced from the thermophillic bacteria, Alicyclobacillus acidoterrestris, in pineapple juice

International audienc