Determination of Origin of Commercial Flavored Rapeseed Oil by the Pattern of Volatile Compounds Obtained via GC–MS and Flash GC Electronic Nose

Flavored rapeseed oil (FRO) is a typical hot‐pressed oil and is widely consumed in China due to its strong characteristic flavor and intensive color. In this study, volatile profiles of 33 representative commercial rapeseed oils in China are characterized by gas chromatography‐mass spectrometry (GC‐MS) and flash gas chromatography (GC) electronic nose system. 51 volatile compounds are identified and the nitriles (methallyl cyanide and 5‐cyano‐1‐pentene), aldehydes (nonanal, 3‐furaldehyde, and 5‐methyl‐2‐furancarboxaldehyde), alcohols (1,5‐hexadien‐3‐ol, 2‐furanmethanol, and phenylethyl alcohol), and pyrazines (2,5‐dimethyl‐pyrazine and 2,6‐dimethyl‐pyrazine) are the major volatile compounds in FROs. Glucosinolate degradation products account for the highest proportion of these volatiles, which are found to have a positive correlation with the erucic acid content (R² = 0.796, p < 0.01). FRO from Sichuan province in the southwest of China can be characterized by the obvious distinctions in flash GC electronic nose combined with principal component analysis, which indicates that the flash GC electronic nose can be used as a promising method to identify the origins of FRO. Practical Applications: This work is helpful for expanding the knowledge of volatiles of commercial flavored rapeseed oil. The data can also serve as a basis for the quality assessment of hot‐pressed rapeseed oil. Meanwhile, the flash GC electronic nose combined with principal component analysis can be used as a promising method for the classification of flavor rapeseed oil production areas.     

Effect of Resin Types and Antioxidants on Release of Off-Flavor From HDPE Bottles

The effects of three types of high-density polyethylene (HDPE) resins (A, B, and C) and three antioxidants (vitamin E, Irganox 1010, and BHT) on the release of off-flavor (including off-odor and off-taste) from blow-molded HDPE bottles were investigated using sensory analysis and gas chromatography/mass spectrometry (GC/MS) analysis. Overall the sensory study showed that off- flavor intensity was affected by both resin type and antioxidant. Resin A bottles yielded less off-flavor compared to resin B or C bottles. Vitamin E containing bottles yielded less off-flavor compared to Irganox 1010 or BHT containing bottles for resins A and B; however, the antioxidants have almost the same effect on resin C. The GC/MS study identified more than 60 volatile compounds released from the bottles, ranging from C₅ to C₂₀, which belonged to the groups of n-alkane, 1-alkene, aldehyde, ketone, phenolic, olefin, and paraffin—among them aldehydes and ketones were the most important due to their very low odor thresholds. Resin A bottles yielded less aldehyde and ketone compared to resin B or C bottles. Vitamin E containing bottles yielded less aldehydes and ketones compared to bottles containing Irganox 1010 or BHT. There was a general consistency between the sensory and GC/MS data. The aldehyde and ketone concentration was linearly correlated reasonably well to odor (R ² = 0.78) and taste scores (R ² = 0.67). Another study was also conducted, which shows vitamin E has smaller reduction in melt flow index due to blow molding compared to Irganox 1010 or BHT.     

The use of electronic and human nose for monitoring rapeseed oil autoxidation

This work was aimed at assessing the effectiveness of the electronic nose to monitor off‐flavor associated with lipid oxidation as a supplementary tool to human sensory panel assessment. Therefore, correlations between electronic nose and sensory analysis were determined. Also GC analyses and chemical analyses of oil samples were run to characterize the analyzed samples with well‐described parameters. Refined rapeseed oil was subjected to an accelerated storage test for 12 days at 60 °C and to an ambient temperature storage test in which it was stored in retail plastic bottles for up to 6 months. PCA of electronic nose data samples stored at an elevated temperature was related to PCA of sensory analysis, and similarities in sample clustering were observed. For samples stored at room temperature, the human panel showed greater sensitivity than the electronic nose. Prediction models based on PLS of electronic nose data were able to predict the sensory quality changes during storage at elevated and room temperature, ranging from 0.721 to 0.989 and from 0.849 to 0.881 (p <0.05), respectively. PV and p‐AV were well predicted on the basis of both electronic nose (0.989, 0.998 for elevated temperature; 0.907, 0.881 for room temperature) and sensory analysis data (0.973, 0.993 for elevated temperature; 0.939, 0.886 for room temperature). Applicability of the electronic nose technology to verify sensory and rancidity changes during storage showed to be promising in quality control of oils.     

Volatile compounds of original African black and white shea butter from Tchad and Cameroon

Shea butter is used as an edible vegetable fat in many African countries. It can be utilized as a substitute or complete replacement for cocoa butter in various applications and plays an important role in traditional African medicinal practice. Although detection of volatile compounds by solid‐phase micro‐extraction gas‐chromatography mass‐spectroscopy (SPME‐GC‐MS) is a very reliable and reproducible technique, which can be used as an important part of authenticity checking, production monitoring and contamination detection, no published data about volatile compounds of shea butter are available so far. In this investigation, the characteristic volatiles in the headspace of original African shea butter samples were identified by using SPME‐capillary‐GC coupled to a mass selective detector. Almost 100 different volatile components were identified, e.g. fatty acids, saturated and unsaturated aldehydes and ketones, terpenes, and typical Maillard reaction products such as methylfuranes and pyrazines. Furthermore, the samples have been olfactorily evaluated by a panel of professional flavorists and trained analytical chemists. It can be stated that variations in processing conditions of shea butter result in considerable differences in the composition of headspace volatiles, detected by SPME‐GC‐MS and human olfaction.     

Identification of volatile flavor compounds in roasted coconut

Heating of coconut leads to browning and development of fine roasted flavor. Flavor studies were carried out with control and heated samples of conconut. Gas chromatography (GC) and GC/mass spectrometry analyses of the basic, neutral and acid fractions of flavor, isolated by hydrodistillation and selective extraction, showed the presence of pyrazines and other heterocyclic compounds in heated samples. These compounds contribute to the overall roasted flavor. Twenty pyrazines were identified in roasted coconut, which included pyrazine, methyl pyrazine, dimethyl pyrazines, ethyl methyl pyrazines, vinyl pyrazine and isopropyl pyrazine. Pyrazine content increased with temperature. In addition to these compounds,δ-lactones, esters, ketones and fatty acids were present in control and heated samples of coconut.     

Fatty Acids and Flavor Components in the Oil Extracted from Golden Melon Seeds

For complete utilization of raw materials and edible oil production, the oil from golden melon seeds (GSs) is extracted via the cold-pressing, hot-pressing, and ultrasound-assisted aqueous enzymatic extraction (AEE), and the fatty acid composition, and nutritional value of the extracted GS oils (GSOs) are analyzed. The volatile compounds present in the GSOs are determined using gas chromatography–mass spectrometry. The aroma profiles of different GSO samples are further distinguished by using an electronic nose. A total of 16 fatty acids are identified in the GSO samples, with atherogenic, thrombogenic, and nutritive value indices ranging from 0.142–0.151, 0.366–0.403, and 5.019–5.299, respectively. Moreover, 43 volatile compounds, including esters, hydrocarbons, alcohols, ketones, pyrazines, and aldehydes are identified. The cold-pressed GSO presents fresh and fruity flavors, while the hot-pressed GSO presents roasted, nutty, fatty, and fruity flavors, and the GSO obtained via AEE presents fatty and fruity flavors. The acid and peroxide contents of these oil samples are 0.69–079 mg g⁻¹ and 5.17–5.79 mmol kg⁻¹, respectively. The results indicate that the extraction method affects the fatty acid composition, flavor components, and physiochemical properties of the GSO. This study may help promote the development of edible GSO. Practical applications: With high demand for edible oils, it is of great significance to find natural edible oils from different sources. The oil in golden melon seeds is extracted by different methods. Their fatty acid composition and flavor components are analyzed. The GSO extracted via AEE method is rich in fatty acids composition. This work would guide the development of an edible GSO and increase the value of golden melon.     

Fish oil sensory properties can be predicted using key oxidative volatiles

The high level of PUFA in fish oil, primarily eicosapentaenoic acid (EPA) and DHA result in rapid oxidation of the oil. Current methods used to assess oxidation have little correlation with sensory properties of fish oils. Here we describe an alternative method using solid phase microextraction (SPME) combined with GC‐MS to monitor volatile oxidation products. Stepwise discriminant function analysis (DFA) was used to classify oils characterized as acceptable or unacceptable based on sensory analysis; a cross‐validated success rate of 100% was achieved with the function. The classification function was also successfully validated with tasted samples that were not used to create the method. A total of 14 variables, primarily aldehydes and ketones, were identified as significant discriminators in the classification function. This method will be useful as a quality control method for fish oil manufacturers. Practical applications: This paper describes an analytical method that can be used by fish oil manufacturers for quality control purposes. Solid phase microextraction and GC‐MS were used to monitor volatile oxidation products in fish oil. These data, combined with results of analyses by a sensory panel, were used to create a function that classified fish oil samples as acceptable or unacceptable. The volatile oxidation products used to in the function were primarily aldehydes and ketones. This method can be used by fish oil manufacturers as an alternative to expensive sensory panels.     

Changes in fatty acids and volatile components in mackerel by broiling

Mackerel is known to be a rich source of omega‐3 family PUFAs. The acid value and conjugated dienoic acid value of mackerel, known as indices of oxidation, were determined. Fatty acids in both raw and broiled mackerels were analyzed by GC. PUFAs and saturated fatty acids were observed at a low level in broiled mackerel, possibly as a result of thermal degradation of the lipids. In addition, volatile components in mackerel extracted by solvent‐assisted flavor evaporation were analyzed by GC‐MS. In total, 38 volatile components were detected in raw mackerel, whereas 53 volatiles were found in broiled mackerel. Hydrocarbons and methyl‐ and/or ethyl‐substituted benzenes were quantitatively dominant. Levels of aldehydes and alcohols were significantly enhanced in broiled mackerel, as was the level of benzothiazole, which possibly forms as a result of the condensation of thermal degradation products from amino acids and/or proteins, and lipids.     

Bitter off‐taste in stored cold‐pressed linseed oil obtained from different varieties

Freshly pressed linseed oil shows a delicate nutty flavor. However, after only 1 day of storage, a bitter off‐taste develops. It is caused mainly by the formation of a cyclic octa‐peptide named cyclolinopeptide E (CLE) containing the oxidized amino acid methionine. A simple and fast determination by solid‐phase extraction and high‐performance liquid chromatography with UV detection has been developed in order to measure the formation of this cyclic peptide during storage in correlation with the increasing bitter off‐taste of the oil, which was determined by a sensory panel. The development of this bitter off‐taste was analyzed in several oils prepared from linseed of a single variety from seeds obtained during a growing test. Highest bitterness was perceived in oil from the variety Eurodor, corresponding to CLE contents of 925 mg/kg, and lowest bitterness was perceived in oil from the variety Baladin, corresponding to a CLE content of 485 mg/kg. In some varieties, additional bitter compounds might be present in significant amounts.     

Azines from one-pot reaction of thiosemicarbazones

Thermolysis and/or microwave irradiation of thiosemicarbazones gave the corresponding isothiocyanates, which on addition of either activated nitriles or aldehydes furnished various types of azines. The mechanism was discussed. The structures of products were proved by MS, IR, NMR, and elemental analyses.     

Detection of adulteration of sesame and peanut oils via volatiles by GC × GC–TOF/MS coupled with principal components analysis and cluster analysis

The method of headspace coupled with comprehensive two‐dimensional GC–time‐of‐flight MS (HS‐GC × GC–TOF/MS) was applied to differentiate the volatile flavor compounds of three types of pure vegetable oils (sesame oils, peanut oils, and soybean oils) and two types of adulterated oils (sesame oils and peanut oils adulterated with soybean oils). Thirty common volatiles, 14 particular flavors and two particular flavors were identified from the three types of pure oils, from the sesame oils, and from the soybean oils, respectively. Thirty‐one potential markers (variables), which are crucial to the forming of different vegetable oil flavors, were selected from volatiles in different pure and adulterated oils, and they were analyzed using the principal component analysis (PCA) and cluster analysis (CA) approaches. The samples of three types of pure vegetable oil were completely classified using the PCA and CA. In addition, minimum adulteration levels of 5 and 10% can be differentiated in the adulteration of peanut oils and sesame oils with soybean oils, respectively. Practical applications: The objective was to develop one kind of potential differentiated method to distinguish high cost vegetable oils from lower grade and cheaper oils of poorer quality such as soybean oils. The test result in this article is satisfactory in discriminating adulterated oils from pure vegetable oils, and the test method is proved to be effective in analyzing different compounds. Furthermore, the method can also be used to detect other adulterants such as hazelnut oil and rapeseed oil. The method is an important technical support for public health against profit‐driven illegal activities.     

一种鸡肉香精的分析与制备

利用顶空固相微萃取法(HS-SPME)提取鸡肉香精中的挥发性成分,并结合气相色谱-质谱联用技术(GC-MS)分析其挥发性成分。结果在鸡肉香精中鉴定出34种挥发性成分,主要包括醛、醇、酮、吡嗪、噻唑、呋喃等化合物。根据测定出的香气成分调配出了一款香气纯正的鸡肉香精。     

Furans and other volatile compounds in ground roasted and espresso coffee using headspace solid-phase microextraction: Effect of roasting speed

The profile of major classes of furanic compounds, as well as other volatile compounds, was evaluated by headspace solid-phase microextraction GC/MS in Arabica ground coffee roasted at three speeds, and in their respective espresso coffees. A total of 113 and 105 volatile compounds were respectively identified in ground coffee and espresso coffee. They were clustered in the following chemical classes: furans, pyrroles, pyridines, pyrazines, ketones, hydrocarbons, aldehydes and others. Results from Principal Component Analysis (PCA) using the data of major volatile class as variables showed that the levels (expressed as relative percentage of total peak area) of furans and pyrroles were higher in espresso samples, whereas those of pyrazines and ketones were higher in ground samples. Slow roasting speed favoured pyridines formation, while medium and fast roasting speed favoured ketones formation. The most representative furanic compound in ground samples was furfuryl alcohol, followed by furfuryl acetate, 2-furfural, 2-methylfuran and 5-methylfurfural. In espresso samples, the levels of 2-methylfuran, 2-furfural, furfuryl formate, 5-methylfurfural and furfuryl acetate were largely increased while the proportion of furfuryl alcohol was strongly reduced in comparison to ground coffee. High roast speed increased formation of 2-furfural and 5-methyl furfural in espresso coffee.     

自制吸附萃取搅拌棒结合气相色谱嗅觉计（GC/O）、气质联用仪（GC/MS）分析肉味香精呈香组分

采用自制吸附萃取搅拌棒对肉味香精呈香组分进行提取,利用热脱附仪进样,结合气相色谱嗅觉计联用（GC/O）、气质联用（GC/MS）双重定性方式,令组分富集率更高,检测结果更加真实、客观地反映出香精的香气组成。为高级香精的调配及仿香工作提供有力依据。实验仪器采用在色谱柱出口安装＂石英三通＂进行1∶1分流,样品被同时引入质谱和嗅觉计,避免了单一定性方法存在的不足。其中,两种方法共同检出的物质31种,仅GC/O检出的物质24种,仅GC/MS检出的物质26种。     

Characterization of Aroma-Active Compounds in Iranian cv. Mari Olive Oil by Aroma Extract Dilution Analysis and GC–MS-Olfactometry

Aroma, aroma‐active compounds and fatty acid profiles of Iranian olive oil obtained from the cv. Mari were investigated for the first time in the current study. Aroma extracts were isolated from the oil by using a purge and trap extraction system and their compositions were analyzed by gas chromatography‐mass spectrometry‐olfactometry (GC–MS‐O). A total of 35 aroma compounds comprising alcohols, aldehydes, acids, esters, ketones, terpenes and volatile phenols were identified and quantified in the assayed samples. Aldehydes were present at the highest levels, followed by ketones and alcohols. (E)‐2‐Hexenal was quantitatively (1589 µg kg^?1) the main aroma compound in the analyzed oils, followed by hexanal and (E)‐2‐heptenal. The aroma‐active volatiles were elucidated in the aromatic extract by applying aroma extract dilution analysis (AEDA). The results of AEDA revealed 17 aroma‐active compounds. Under these condition it was possible to completely identify 16 of these compounds. Regarding to the flavor dilution (FD) factor, the most potent odorants with the highest FD factor were (E)‐2‐hexenal (512), followed by hexanal, 6‐methyl‐5‐hepten‐2‐one, (E)‐2‐decenal and one unknown compound (LRI = 1871). The fatty acid profile of the tested oils was composed of thirteen compounds. Oleic acid was the main fatty acid (76.01 %) followed by palmitic acid.     

国内外低焦油烤烟型卷烟中性香味成分的分析比较

将国内外5种（国外1种,国内4种）低焦油烤烟型卷烟烟丝经同时蒸馏萃取、GC、GC／MS分析测试,对低焦油烤烟型卷烟烟丝29种中性香味成分进行了分析研究。国内外卷烟烟丝的常规化学成分也进行了测试比较。结果发现,国产烤烟型卷烟挥发性、半挥发性中性成分总量、酮类成分总量、醇类成分总量比国外烤烟型卷烟低,醛类成分总量、酯类成分总量比国外高。4种国产烤烟型卷烟烟丝重要中性香味成分中均比国外烤烟型卷烟低10％以上的有：苯乙醛、糠醇、苯甲醇、六氢金合欢基丙酮和2-甲氧基4-乙烯基苯酚;均高于10％的有：糠醛、亚麻酸甲酯等。     

分子蒸馏处理香料烟浸膏制备烟用香料

为了更好地精制富集烟草特征香味成分,采用分子蒸馏技术对溶剂法制备的香料烟浸膏进行分离,并对馏分进行GC/MS分析。GC/MS结果显示,在不同温度段,香料烟浸膏致香成分得到富集,特别是40～60℃馏分中香料烟重要香味成分茄酮达到了17%。评吸结果显示：原香料烟提取物能增香及提高香气质,但残留明显。经分子蒸馏处理后,40℃以下馏分香气质较好,香气量不足,余味舒适;40～60℃馏分香气质好,丰富烟香,口腔舒适,改善烟气状态;60～80℃馏分增加香气量,舌面口腔有残留;蒸余物则对烟气增香无明显影响。     

Influence of Storage on Physicochemical and Volatile Features of Enriched and Aromatized Wax Organogels

In this study, virgin olive oil (VOO) organogels were produced with beeswax (BW) and sunflower wax (SW) and enriched with β‐carotene, vitamin D₃ and E as well as aromatized with strawberry, banana, and butter aromas. The physicochemical, thermal, structural, and sensorial properties of the fresh organogel samples were determined. The peroxide values, antioxidant activities, firmness, and volatile compositions of the fresh samples and those stored for 3 months were also determined. The organogels were not only stable, uniform, and homogenous during the storage period but also the added components did not affect the organogel properties. The panel defined three appearance, four texture, three mouthfeel, four aroma, and four flavor terms to describe the organogels sensorially. Moreover, the added aroma (banana, strawberry, and diacetyl‐butter) components of the fresh and stored organogels were quantified by GC/MS‐SPME. In conclusion, these results demonstrated that beeswax and sunflower wax are very suitable to preserve the aromatic characteristics of these types of spreadable products.     

UHT脱脂纯牛奶感官评价和电子鼻分析相关性研究

选取四种市售不同品牌的UHT脱脂纯牛奶作为研究对象,通过感官描述性分析和电子鼻技术对其风味属性进行评价。采用主成分分析(PCA)和聚类分析(CA)结合偏最小二乘回归法(PLSR)法将电子鼻传感器性能和感官属性进行相关性分析。结果表明样品奶油味及脂质感评分均较低;电子鼻的十个传感器对四个样品的区分效果良好;基于感官属性和传感器响应值的PLSR分析建立的相关性模型,能够很好地解释感官属性和传感器响应值的相关性,反映脱脂纯牛奶样品的整体信息。本文结合两种技术方法,弥补了人工感官评价存在的主观性与智能感官分析的局限性影响,旨在为后续改善脱脂纯牛奶风味提供技术参考。