Simultaneous Distillation Extraction Research Articles

Studies on the fishy odour removal and physicochemical properties of gelatin from Nile tilapia (<I>Oreochromis niloticus</I>) skin

Nile tilapia (Oreochromis niloticus) aquaculture is expanding throughout the world,most notably in China. According to the statistics of FAO,annual China’s production of tilapia by 2008 had risen to nearly 1.2 million tons,which accounts for about 50% of tilapia production in the world. During processing of tilapia to fillets,large quantities of the by-products such as skin are produced. On one hand,collagen contents in tilapia skins are rich. On the other hand,the bovine spongiform encephalopathy (BSE) episode,as well as religious concerns,has led to intensive research to identify and develop alternatives to mammal-derived gelatin. Therefore,tilapia skin can be a good resource of extracting gelatin. However,gelatin extraction from tilapia skin usually had a strong fishy odour,which would limit its utilization. In order to be applied to food and pharmaceutical industries,some methods must be adopted to make the gelatin odorless. In the present study,methods of active carbon absorption,yeast and lactobacillus fermentation were used to remove fishy odour in the gelatin,in which their roles to diminish fishy odour were compared with each other by sensory analysis. And the effects of active carbon absorption conditions on the transmittance and sensory scores of the gelatin solution were studied by orthogonal experiments. After removing fishy odour,the physicochemical properties of the gelatin were studied and its volatile components were evaluated by simultaneous distillation-extraction (SDE) and gas chromatography-mass spectrometry (GC-MS). Sensory analysis showed that the effects of fishy odour removal of gelatin were significantly different among methods of active carbon absorption,yeast and lactobacillus fermentation (P0.05). Among these methods,the best one was active carbon absorption. The results of orthogonal experiment indicated that the optimal conditions were the ratio of active carbon addition to 5% (w/v) gelatin solution 1.5% (w/v),and incubated at 40 ℃ for 30 min. After removal treatment,fishy odour in the tilapia skin gelatin was barely detectable. The content of crude protein in the gelatin was 91.3% and its gel strength was high up to 301 g. The transmittance of the tilapia skin gelatin solution was higher than before treatment,and the content of water-undissolved matter was diminished. A total of 33 volatile components in tilapia skin gelatin solution before removing fishy odour were detected by simultaneous distillation-extraction (SDE) and gas chromatography-mass spectrometry (GC-MS). The volatile compounds of the gelatin solution were predominantly esters,followed by alcohols,ketones and olefines. After removing fishy odour,a total of volatile components in gelatin solution have been diminished to 26 kinds,which were mainly olefines and ketones. The research shows that active carbon absorption appears as a suitable technique to remove fishy odour in tilapia skin gelatin and to improve their physicochemical properties. So,it can be used for industrial production of fishy odour free tilapia skin gelatin.

Isolation and Identification of Volatile Components in <i>Tempe</i> by Simultaneous Distillation-Extraction Method by Modified Extraction Method

An isolation and identification of volatile components in temps for 2, 5 and 8 days fermentation by simultaneous distillation-extraction method was carried out. Simultaneous distillation-extraction apparatus was modified by Muchalal from the basic Likens-Nickerson's design. Steam distillation and benzena as an extraction solvent was used in this system. The isolation was continuously carried out for 3 hours which maximum water temperature In the Liebig condenser was 8 °C. The extract was concentrated by freeze concentration method, and the volatile components were analyzed and identified by combined gas chromatography-mass spectrophotometry (GC-MS). The Muchalal's simultaneous distillation extraction apparatus have some disadvantage in cold finger condenser, and it's extractor did not have condenser. At least 47, 13 and 5 volatile components were found in 2, 5 and 8 days fermentation, respectively. The volatile components in the 2 days fermentation were nonalal, ɑ-pinene, 2,4-decadienal, 5-phenyldecane, 5-phenylundecane, 4-phenylundecane, 5-phenyldodecane, 4-phenyldodecane, 3-phenyldodecane, 2-phenyldodecane, 5-phenyltridecane, and caryophyllene; in the 5 days fermentation were nonalal, caryophyllene, 4-phenylundecane, 5-phenyldodecane, 4-phenyldodecane, 3-phenyldodecane, 2-phenyldodecane; and in the 8 days fermentation were ethenyl butanoic, 2-methy1-3-(methylethenyl)ciclohexyl etanoic and 3,7-dimethyl-5-octenyl etanoic.

The Effects of Maturity on Chilli Pepper Volatile Components Determined by SDE, GC-MS and HPLC

The volatile components of a Chinese chilli pepper (Capsicum annuum L. var. longum Sendt) were identified at different levels of ripeness. The peppers at the green, ripening, and full color stages were investigated by simultaneous distillation extraction (SDE) combined with gas chromatography and mass spectrometry (GC-MS). Principal component analysis (PCA) was used to analyze the main factors at each of the stages studied. Eighty-one volatile components were identified and quantified in this study. Twenty-two compounds were found at the green stage, forty-four at the ripening stage, and sixty-one at the full color stage. Qualitative and quantitative discrepancies were observed at the different levels of ripeness. Hexanal, 2-hexenal and propanoic acid-2-methyl-hexyl ester were the most abundant components at the green stage, while 2-pentanol was important at the ripening stage, and 3-hexen-1-ol was related to the full color stage.

GENERATION OF MEAT-LIKE VOLATILES FROM CYSTEINE, GLUCOSE AND SERINE MODEL SYSTEM AND ITS ANTIOXIDANT ACTIVITY

Reaction between Cysteine, Glucose and Serine was carried out to study the volatiles formed via Maillard reaction and their antioxidant activity. The simultaneous distillation–extraction technique was used for trapping the volatile components followed by GC–MS analysis. Thirty Six compounds were identified with the predominance of carbonyls and sulfur–containing compounds in the volatiles of this model system. Sensory evaluation was performed for the model system product according to the International Standard Methods (ISO). The results showed a high increase in roasted and burnt meat attributes. The sensory results of the model system product were confirmed by the presence of high concentrations of some volatile compounds having meat–like aroma such as 2-methyl-3-furanthiol and 2-furylmethanethiol attributes and remarkable increase in the like– roasted meaty aroma. The radical scavenging activity of cysteine, glucose and serine model system was quantified spectrophotometrically, using DPPH radical. The activity of the model system product was found to be slightly lower than that of gallic acid and BHA, but it was much higher than that of cinnamic acid (200 ppm. for each). A highly antioxidative activity was recorded by the model system which may be due to the presence of some compoundssuch as 2-furylmethanethiol, 2-acetylthiazole, 4-hydroxy-5-methyl-3(2H)-furanone.

Essential Oils from Six Herbal Plants for Biocontrol of the Maize Weevil

Essential oils from sweet basil (Ocimum basilicum L.), holy basil (O. americanum L.), hairy basil (O. tenuiflorum L.), lime (Citrus aurantifolia Swingle), kaffir lime (C. hystrix DC.), and clove (Eugenia caryophyllus L.) were isolated by simultaneous distillation extraction. Toxicity assays against the maize weevil (Sitophilus zeamais Motschulsky) using 30 to 120 μL oil extract from the six plants on 70-mm-diameter filter paper discs resulted in 100% weevil mortality within the 5-h assay period. On rice samples, sweet basil oil extract was the most effective, resulting in 96% to 100% mortality regardless of oil extract volume on the first day during the 5-day assay period. Probit analysis showed that sweet basil oil extract applied on grains had four to five times lower LD50 (lethal dose to kill 50% of the weevils) and two to three times lower LD99 values than the remaining oil extracts. Repellency assay using 1 to 8 μL oil extract showed a different trend, because hairy basil was the most effective among treatments. Based on the effective control of the maize weevil by the oil extracted from herbal plants, such oil extracts could be useful in stored agricultural products and plant protection and reduce the risk associated with synthetic insecticides.

A Comparison of Volatile Components of Setomi with Its Parent Cultivars

The citrus fruit Setomi is a hybrid of Yoshiura ponkan (Citrus reticulate Blanco) and Kiyomi (Citrus unshiu Mrcov. x Citrus sinensis Osbeck). The essential oils from the peel of Setomi and its parent cultivars were obtained by a simultaneous distillation extraction technique. Comparing the essential oils of Setomi and its parent cultivars, it was found that the oil in the peel of Setomi consisted of characteristic aroma components from each parent cultivar. The principal component analysis of data, obtained with an electronic nose, indicated that the odor quality of Setomi was different from those of the parent cultivars.

Accelerated solvent extraction for GC-based tobacco fingerprinting and its comparison with simultaneous distillation and extraction

An accelerated solvent extraction (ASE) procedure has been developed as a pretreatment method for chemical fingerprinting of volatile and semi-volatile components in cut tobacco. The ASE extraction conditions including temperature, operation pressure and extraction cycles were optimized to maximize extraction yield. The method was validated with repeatability, recovery and linearity. Compared with simultaneous distillation extraction (SDE), ASE provides higher extraction yields, less extraction time, lower solvent consumption and less labor time, and is more suitable for tobacco sample preparation. A typical ASE extract was analyzed by gas chromatography/time-of-flight mass spectrometry (GC-TOFMS). A total of 305 components with signal-to-noise ratio higher than 100 were tentatively identified by NIST05 and Wiley database. Finally, 36 cigarette samples from six cigarette brands were analyzed using the developed chemical fingerprinting method. Partial least squares-discriminant analysis shows good discrimination of different cigarette brands. The results indicate that ASE method can serve as high-throughput sample preparation technique for cigarette chemical fingerprint analysis.

Volatile compounds from Rosmarinus officinalis L. and Baccharis dracunculifolia DC. Growing in southeast coast of Brazil

Chemical composition of leaf volatiles of Rosmarinus officinalis and Baccharis dracunculifolia cultured in Southeast of Brazil has been characterized by GC/MS after simultaneous distillation-extraction. The main components in volatiles of these species showed in common α-pinene, myrcene, 1,8 cineole and camphor. Camphor was the major component among volatiles of B. dracunculifolia and R. officinalis with concentrations exceeding 25%. B. dracunculifolia volatiles possessed more sesquiterpenes (21.4%) than R. officinalis (16.7%), such as caryophyllene (1.9%) and α-humulene (0.4%). Lower concentrations of nerolidol and spathulenol were achieved in volatiles of B. dracunculifolia. Considering both species, there was a predominance of monoterpenes.

Characterisation of Chamomile Volatiles by Simultaneous Distillation Solid-Phase Extraction in Comparison to Hydrodistillation and Simultaneous Distillation Extraction

A new method for complete separation of steam-volatile organic compounds is described using the example of chamomile flowers. This method is based on the direct combination of hydrodistillation and solid-phase extraction in a circulation apparatus. In contrast to hydrodistillation and simultaneous distillation extraction (SDE), an RP-18 solid phase as adsorptive material is used rather than a water-insoluble solvent. Therefore, a prompt and complete fixation of all volatiles takes place, and the circulation of water-soluble bisabololoxides as well as water-soluble and thermolabile en-yne-spiroethers is inhibited. This so-called simultaneous distillation solid-phase extraction (SD-SPE) provides extracts that better characterise the real composition of the vapour phase, as well as the composition of inhalation vapours, than do SDE extracts or essential oils obtained by hydrodistillation. The data indicate that during inhalation therapy with chamomile, the bisabololoxides and spiroethers are more strongly involved in the inhaling activity than so far assumed.

Comparison of isolation methods for the determination of buckwheat volatile compounds

Five different isolation techniques were combined with gas chromatographic–mass spectrometric determination of aroma compounds from buckwheat: dynamic headspace (DHS) with cryotrapping or sorbent trapping, solid-phase microextraction (SPME), headspace sorptive extraction (HSSE), solvent extraction (SE) and simultaneous distillation–extraction (SDE). Optimisation of each technique is presented, as well as comparison of the chemical profiles obtained by them. Solvent extraction with methanol resulted in the isolation of rather polar and less volatile compounds and was deemed least suitable for the odour-active compounds. Only SPME with DVB/CAR/PDMS fibre was suitable for the isolation of highly volatile compounds in a wider polarity range. DHS extracted the smallest number of compounds, but with the comparable chemical profile as obtained by SDE, which was chosen as the most suitable technique to obtain the aroma compounds of cooked buckwheat. The applied isolation techniques are complementary in their ability to extract a representative aroma profile of buckwheat.

Volatile compounds profile and sensory evaluation of Beninese condiments produced by inocula of Bacillus subtilis

Three Beninese food condiments (ABS1(24h), IBS2(48h) and SBS3(48h)) were produced by controlled fermentation of African locust beans using inocula of pure cultures of Bacillus subtilis, BS1, BS2 and BS3, respectively. Quantitative and qualitative assessments of the volatile compounds in the condiments produced have been performed using the Likens-Nickerson simultaneous distillation-extraction method and GC-MS analysis, followed by a sensory evaluation in comparison with the spontaneously fermented condiments. A total of 94 volatile compounds have been found including 53 compounds identified in relatively high concentrations and were subdivided into seven main groups with the predominance of four major groups: pyrazines, aldehydes, ketones and alcohols. Compared to the spontaneously fermented condiments, volatile compounds identified in controlled fermented condiments have been found in high number and in concentrations which varied according to the inoculum of B. subtilis used. The condiments produced with starter cultures scored significantly (P < 0.05) higher for odour than the spontaneously fermented condiments. But the overall acceptability (7/10) of the two types of condiments was similar. The investigated B. subtilis, BS1, BS2 and BS3 can be considered as potential starter cultures for the fermentation of African locust beans to produce good quality of Beninese food condiments.

Occurrence of odour-causing compounds in different source waters of China

In this study, occurrence of the main odorous compounds in different types of source water in China, including rivers, lakes and reservoirs, were investigated by integrating the methods of flavour profile analysis (FPA) and sensory-GC/MS analysis. Simultaneous distillation extraction (SDE) was chosen as the preconcentration technique while the odour-causing compounds were identified with sensory-GC/MS. It was found that MIB, which is mainly produced by some cyanobacteria and actinomycetes, was one of the most widely distributed odour-causing compounds, regardless of source type. A peak MIB concentration of approximately 170 ng l(-1) was recorded in MY Reservoir in October 2005. Among the nine investigated sites, YH Reservoir in Hebei Province was the only site showing geosmin production. A peak geosmin concentration exceeding 7,000 ng l(-1) was detected in July 2007. In June 2007, a serious taste/odour (T/O) event occurred in Wuxi City, and the offensive flavour was a strong septic or marshy odour caused by dimethyl trisulfide (431 ng l(-1) in finished water). Septic/swampy and earthy/musty odours occurred in source waters of Shanghai and Guangzhou. It was found that dimethyl trisulfide was mainly responsible for the septic/swampy odour and MIB for the earthy/musty one. Dimethyl trisulfide might be an important T/O-causing compound in China.

Changes in volatile compounds of a native Chinese chilli pepper (Capsicum frutescens var) during ripening

SummaryThe objective of this study was to identify the volatile components of a native Chinese chilli pepper (Capsicum frutescens var) at different ripening stages. The peppers at green, breaking and red colour stages were first investigated by simultaneous distillation extraction combined with gas chromatography and mass spectrometry. Principal component analysis was used to visualise the grouping tendencies of the studied stages of pepper. Eighty‐five volatile organic components were identified and quantified in this study. Forty compounds were found at the green stage, fifty‐three at the breaking stage and sixty‐five at the red colour stage. The flavour activity compounds were discovered in Chinese pepper. Qualitative and quantitative discrepancies were observed in different ripening stages. The amount of alkenes and aldehydes increased from 2.762% and 0.120% in green stage to 11.137% and 14.485% in colours’ stage. The content of Alcohols decreased from 30.169% to 23.698%. Only, the aromatic compound disappears during maturity. Ketones enhanced from 0.983% to 2.693%. Esters were always reducing.

The chemical relationship between the scent features of goldenrod ( Solidago canadensis L.) flower and its unifloral honey

The marker compounds of Solidago origin in goldenrod flower and honey have been investigated. After Likens–Nickerson simultaneous distillation–extraction (SDE) the extracts were dehydrated and concentrated, then thoroughly analysed by GC–MS. Among the common compounds of the flower and honey, germacrene-D proved to be the most suitable for identification of the goldenrod origin. The presence of this constituent creates a unique sesquiterpene spectrum in aroma extracts of the flower and honey, making the recognition more precise and reliable. The aroma structure examinations revealed the characteristic scent pictures of the flower and its unifloral honey and proved that no direct “morphological” similarity/identity exists between the aromaspectra of the two fragrance extracts (honey contra flower), except the presence of the common compounds. The results of the investigations covering the 2005 and 2006 apiarian seasons showed excellent repeatability and reliability.

Analysis of volatile compounds of wild gilthead sea bream ( Sparus aurata) by simultaneous distillation–extraction (SDE) and GC–MS

The volatile compounds of wild gilthead sea bream ( Sparus aurata) were analyzed by sensory and instrumental analyses. Simultaneous distillation and extraction (SDE) with dichloromethane were used for extraction of volatile components. According to sensory analysis, the aromatic extract obtained by SDE was representative of sea bream odour. A total of 46 compounds were identified and quantified in sea bream. Aldehydes and alcohols were the most dominant volatiles in sea bream, as they accounted for the largest proportion. Hexanal, heptanal, nonanal, ( Z)-4-heptenal, octanal, ( E)-2-nonenal, decanal, benzenacetaldehyde, ( E, E)-2,4-decadienal, 1-octen-3-ol and ( E)-1,5-octadien-3-ol were potent aroma compounds on the basis of odour activity values (OAVs). Within these, decanal (OAV: 1110) and ( E)-2-nonenal (OAV: 447.5) were the most powerful contributors to the aroma of the sea bream.

An integrated simultaneous distillation–extraction apparatus for the extraction of essential oils from herb materials and its application in Flos Magnoliae

A large number of herb materials contain essential oils with extensive bioactivities. In this work, an integrated simultaneous distillation-extraction (ISDE) apparatus was developed. To demonstrate its feasibility, the performance of ISDE was evaluated for the extraction of essential oil from Flos Magnoliae and compared with conventional techniques including steam distillation (SD) and simultaneous distillation-extraction (SDE). According to the product yield, the time consumed and the composition of oil, the essential oils isolated by ISDE were better than that obtained by SD and similar to those obtained by SDE. ISDE was also better than SDE due to its simple operation and lower consumption of energy and organic solvent.

Comparison of extraction methods for volatile compounds of Muscat grape juice

Typical flavour of Muscat d’Alexandrie wines is mainly due to volatile compounds coming from grapes of this variety. Therefore, the choice of grapes is crucial to obtain musts with a great aromatic potential, which will contribute to the final aroma of wines derived from those musts. In this study, three sampling techniques, liquid–liquid extraction (LLE), solid phase extraction (SPE) and simultaneous distillation-extraction (SDE), were compared for the analysis of volatile compounds in Muscat grape juice. Results showed that although the three techniques can be recommended for the quantitative analysis of volatile compounds from musts, LLE and SPE are better sample preparation techniques than SDE, mainly for determination of polar compounds such as acids or alcohols.

Occurrence of 2,2,4-trimethyl–1,3-pentanediol monoisobutyrate (Texanol®) in foods packed in polystyrene and polypropylene cups

After simultaneous distillation–extraction (SDE) of foods packed in polystyrene (n = 77) and polypropylene cups (n = 42) from 61 different suppliers, coupled capillary gas chromatography–mass spectrometric (HRGC–MS) analyses indicated the presence of diastereomers of 2,2,4-trimethyl–1,3-pentanediol monoisobutyrate (TMPD-MIB; Texanol®), a known coalescent of paints and printing inks. The contaminant was found in 55 and 50% of the polystyrene and polypropylene packed samples, respectively. Amounts ranged 1.2–64.5 µg kg−1 in polystyrene cups (average 25.1 µg kg−1) and 0.9–45.7 µg kg−1 in polypropylene cups (average 10.8 µg kg−1). The origin of Texanol® in the printed plastic cups was demonstrated by separate HRGC–MS analysis, showing amounts in the higher µg kg−1 range. In addition, the presence of two pairs of enantiomers, both found to be racemic by enantioselective multi-dimensional gas chromatography–mass spectrometry (enantio-MDGC–MS), excluded it being of natural origin. The detection limit of overall procedure (DLOP) and the reliable quantification limit (RQL) were 0.2 and 0.9 µg kg−1, respectively. As the diester, 2,2,4-trimethyl–1,3-pentanediol diisobutyrate (TXIB), is on the EU list of regulated substances (restricted to single-use gloves only) with a migration limit of 5 mg kg−1 in food and is metabolised rapidly by hydrolysis, the observed migration of the monoester Texanol® at the µg kg−1 level poses no risk of adverse effects.

Development of a Chromatographic Fingerprint of Tobacco Flavor by Use of GC and GC-MS

A new chromatographic fingerprinting method has been established for quality control of tobacco flavor. Three different extraction techniques, simultaneous distillation extraction (SDE), liquid–liquid extraction, and solid-phase microextraction were evaluated for isolation of the components of interest. After comparison of their performance, a combination of SDE and GC-MS was used for simple, reliable, and reproducible development of a chromatographic fingerprint of tobacco flavor. Twelve samples of the flavor from different batches were used to establish the fingerprint. Thirty-nine volatile components of the tobacco flavor samples, accounting for 86.54% of the total content, were identified and quantified. The 12 samples had 28 peaks in common. The method of fingerprint analysis was then validated on the basis of the relative retention times and relative peak areas of the common peaks, sample stability, and similarity analysis. The similarities of the 12 samples of tobacco flavor were >0.80, showing that samples from different batches were, to some extent, consistent. The chromatographic fingerprint developed was successfully used to differentiate tobacco flavor samples from tobacco extract prepared from tobacco leaf, both by similarity comparison and by principal-components projection analysis. The method can be used for quality control of tobacco flavor.

Simultaneous Distillation-Extraction, Hydrodistillation and Static Headspace Methods for the Analysis of Volatile Secondary Metabolites of Alpinia zerumbet (Pers.) Burtt et Smith. from Southeast Brazil

Alpinia zerumbet (Zingiberaceae) is cultivated in several tropical areas. It has ahigh value all over the world as a spice in culinary preparations and for its medicinal properties. Thecomposition of the essential oil obtained by simultaneous distillation-extraction (SDE) andhydrodistillation (HD) from fresh leaves of A. zerumbet was analyzed by GC-MS. In both samples themain constituents were terpinen-4-ol, 1,8-cinole, sabinene and λ-terpinene together with caryophylleneand caryophyllene oxide sesquiterpenes. However, individual percentage values of compoundsvaried between the methods. The components camphene (0.3 %), p-2-mentha-4(8)-diene (1.4 %) andtrans-sabinene hydrate (1.0 %) were obtained only by SDE. Static-headspace (S-HS) was for the firsttime used to analyze the aroma from fresh leaves of A. zerumbet. Sabinene, 1,8 cineole and λ-terpinene were the main terpenes detected through S-HS. Flower oil was extracted by HD method,and the major components identified were 1,8 cineole (15.5 %), λ-terpinene (13.1 %) and terpinen-4-ol (42.3 %). There was a predominance of monoterpenes.