Key aroma compounds identified in Cheddar cheese with different ripening times by aroma extract dilution analysis,odor activity value,aroma recombination,and omission

To determine the odor-active compounds in Cheddar cheeses with different ripening times (6, 10, and 14 mo), 39 potent odorants of Cheddar cheeses were identified with a flavor dilution factor range between 1 and 512 by aroma extract dilution analysis. To further determine their contribution to the overall aroma profile of Cheddar cheeses, odor activity values of 38 odorants with flavor dilution factors ≥1 were calculated. A Cheddar cheese matrix was developed to determine the concentrations and the odor thresholds of these key aroma compounds. The result of the aroma recombinant experiment prepared by mixing the key aroma compounds in the concentrations in which they occurred in Cheddar cheeses showed that the overall aroma profile of the recombinant sample was very similar to that of Cheddar cheese. The main different compounds in Cheddar cheese with different ripening time were acetic acid, butanoic acid, dimethyl trisulfide, methional, hexanal, (E)-2-nonenal, acetoin, 1-octen-3-one, δ-dodecalactone, furaneol, hexanoic acid, heptanal, and ethyl caproate. This study could provide important information for researching and developing Cheddar cheese–related products.     

Identification of aroma-active compounds in Cheddar cheese imparted by wood smoke

Cheddar cheese is the most popular cheese in the United States, and the demand for specialty categories of cheese, such as smoked cheese, are rising. The objective of this study was to characterize the flavor differences among Cheddar cheeses smoked with hickory, cherry, or apple woods, and to identify important aroma-active compounds contributing to these differences. First, the aroma-active compound profiles of hickory, cherry, and apple wood smokes were analyzed by solid-phase microextraction (SPME) gas chromatography-olfactometry (GCO) and gas chromatography-mass spectrometry (GC-MS). Subsequently, commercial Cheddar cheeses smoked with hickory, cherry, or apple woods, as well as an unsmoked control, were evaluated by a trained sensory panel and by SPME GCO and GC-MS to identify aroma-active compounds. Selected compounds were quantified with external standard curves. Seventy-eight aroma-active compounds were identified in wood smokes. Compounds included phenolics, carbonyls, and furans. The trained panel identified distinct sensory attributes and intensities among the 3 cheeses exposed to different wood smokes (P < 0.05). Hickory smoked cheeses had the highest intensities of flavors associated with characteristic “smokiness” including smoke aroma, overall smoke flavor intensity, and meaty, smoky flavor. Cherry wood smoked cheeses were distinguished by the presence of a fruity flavor. Apple wood smoked cheeses were characterized by the presence of a waxy, green flavor. Ninety-nine aroma-active compounds were identified in smoked cheeses. Phenol, guaiacol, 4-methylguaiacol, and syringol were identified as the most important compounds contributing to characteristic “smokiness.” Benzyl alcohol contributed to the fruity flavor in cherry wood smoked cheeses, and 2-methyl-2-butenal and 2-ethylfuran were responsible for the waxy, green flavor identified in apple wood smoked cheeses. These smoke flavor compounds, in addition to diacetyl and acetoin, were deemed important to the flavor of cheeses in this study. Results from this study identified volatile aroma-active compounds contributing to differences in sensory perception among Cheddar cheeses smoked with different wood sources.     

基于快速成熟模型的藏灵菇发酵切达干酪挥发性风味物质分析

通过建立快速成熟干酪模型,采用固相微萃取法提取传统藏灵菇发酵的切达干酪模型与商品发酵剂制作的切达干酪模型中挥发性成分,并结合气相色谱-质谱联用技术和气相色谱-嗅闻技术对萃取成分进行鉴定,结果表明醇类和酯类是藏灵菇发酵切达干酪成熟过程中的主要风味物质。藏灵菇发酵切达干酪模型中风味物质的种类和含量都明显高于商业发酵剂制作的切达干酪模型,其中酯类物质的变化最为显著。感官评价和风味分析结果表明,藏灵菇发酵切达干酪模型中酯类和醇类物质种类和含量更为丰富,风味更强,水果香味更浓郁,还具有酒香味。     

Impact of fat reduction on flavor and flavor chemistry of Cheddar cheeses

A current industry goal is to produce a 75 to 80% fat-reduced Cheddar cheese that is tasty and appealing to consumers. Despite previous studies on reduced-fat cheese, information is critically lacking in understanding the flavor and flavor chemistry of reduced-fat and nonfat Cheddar cheeses and how it differs from its full-fat counterpart. The objective of this study was to document and compare flavor development in cheeses with different fat contents so as to quantitatively characterize how flavor and flavor development in Cheddar cheese are altered with fat reduction. Cheddar cheeses with 50% reduced-fat cheese (RFC) and low-fat cheese containing 6% fat (LFC) along with 2 full-fat cheeses (FFC) were manufactured in duplicate. Cheeses were ripened at 8°C and samples were taken following 2 wk and 3, 6, and 9 mo for sensory and instrumental volatile analyses. A trained sensory panel (n = 10 panelists) documented flavor attributes of cheeses. Volatile compounds were extracted by solid-phase microextraction or solvent-assisted flavor evaporation followed by separation and identification using gas chromatography-mass spectrometry and gas chromatography-olfactometry. Selected compounds were quantified using external standard curves. Sensory properties of cheeses were distinct initially but more differences were documented as cheeses aged. By 9 mo, LFC and RFC displayed distinct burnt/rosy flavors that were not present in FFC. Sulfur flavor was also lower in LFC compared with other cheeses. Forty aroma-active compounds were characterized in the cheeses by headspace or solvent extraction followed by gas chromatography-olfactometry. Compounds were largely not distinct between the cheeses at each time point, but concentration differences were evident. Higher concentrations of furanones (furaneol, homofuraneol, sotolon), phenylethanal, 1-octen-3-one, and free fatty acids, and lower concentrations of lactones were present in LFC compared with FFC after 9 mo of ripening. These results confirm that flavor differences documented between full-fat and reduced-fat cheeses are not due solely to differences in matrix and flavor release but also to distinct differences in ripening biochemistry, which leads to an imbalance of many flavor-contributing compounds.     

Influence of ripening temperature on the volatiles profile and flavour of Cheddar cheese made from raw or pasteurised milk

Cheddar cheeses were made from raw (R1, R8) or pasteurised (P1, P8) milk and ripened at 1°C (P1, R1) or 8°C (P8, R8). Volatile compounds were extracted from 6 month-old cheeses and analysed, identified and quantified by gas chromatography-mass-spectrometry. A detailed sensory analysis of the cheeses was performed after 4 and 6 months of ripening. The R8 cheeses had the highest and P1 the lowest concentrations of most of the volatile compounds quantified (fatty acids, ketones, aldehydes, esters, alcohols, lactones and methional). The R8 and P8 cheeses contained higher levels of most of the volatiles than R1 and P1 cheeses. Ripening temperature and type of milk influenced most of the flavour and aroma attributes. Principal component analysis (PCA) of aroma and flavour attributes showed that P1 and R1 had similar aroma and flavour profiles, while R8 had the highest aroma and flavour intensities, highest acid aroma and sour flavour. The age of cheeses influenced the perception of creamy/milky and pungent aromas. PCA of the texture attributes separated cheeses on the basis of ripening temperature. The R8 and P8 cheeses received significantly higher scores for perceived maturity than P1 and R1 cheeses. The P1 and R1 cheeses had similar values for perceived maturity. In a related study, it was found that concentrations of amino acids and fatty acids were similar in R1 and P1 during most of the ripening period, and R1 and P1 cheeses had low numbers of non-starter lactic acid bacteria (NSLAB). The panel found that ripening temperature, type of milk and age of cheeses did not influence the acceptability of cheese. It is concluded that NSLAB contribute to the formation of volatile compounds and affect the aroma and flavour profiles and the perceived maturity of Cheddar cheese.     

Metabolomics-based component profiling of hard and semi-hard natural cheeses with gas chromatography/time-of-flight-mass spectrometry, and its application to sensory predictive modeling

Gas chromatography/time-of-flight mass spectrometry (GC/TOF-MS) was used to analyze hydrophilic low molecular weight components, including amino acids, fatty acids, amines, organic acids, and saccharides, in cheese, and the sensometric application for practical metabolomic studies in the food industry is described. Derivatization of target analytes was conducted prior to the GC/TOF-MS analysis. Data on 13 cheeses, six Cheddar cheeses, six Gouda cheeses and one Parmigiano-Reggiano cheese, were analyzed by multivariate analysis. The uniqueness of the Parmigiano-Reggiano cheese metabolome was revealed. Principal component analysis (PCA) showed no grouping of the Cheddar cheeses and Gouda cheeses according to production method or country of origin. The PCA loading plot confirms that many amino acids contribute positively to PC1, suggesting that PC1 is closely related to degradation of proteins, and that lactic acid contributed positively to PC2, whereas glycerol contributed negatively to PC2, suggesting that factors regarding degradation of carbohydrates and fats were expressed in PC2. Partial least squares (PLS) regression models were constructed to predict the relationship between the metabolite profile and two sensory attributes, "Rich flavor" and "Sour flavor", which were related to maturation. The compounds that play an important role in constructing each sensory prediction model were identified as 12 amino acids and lactose for "Rich flavor", and 4-aminobutyric acid, ornithine, succinic acid, lactic acid, proline and lactose for "Sour flavor". The present study revealed that metabolomics-based component profiling, focusing on hydrophilic low molecular weight components, was able to predict the sensory characteristics related to ripening.     

甜玉米成熟过程中挥发性风味物质的变化规律

以“仲甜9号”、“珠玉甜8号”、“珠玉甜1号”3 个品种甜玉米为材料,研究甜玉米籽粒成熟过程中挥发性风味物质的变化规律。采用顶空固相微萃取-气相色谱-质谱联用分析技术,结合NIST14质谱数据库比对、保留指数分析、气相色谱嗅闻分析等方法对挥发性风味物质进行鉴定,利用内标法测定其含量,构建甜玉米挥发性风味活性化合物组成谱,评价甜玉米香气品质与特征。结果表明：3 种甜玉米在成熟过程中共检测到61 种挥发性风味物质;成熟度对挥发性风味物质种类和含量有显著影响,随成熟度增加,壬酸乙酯、1-庚醇、1-己醇含量显著下降,苯乙烯、甲苯、乙苯、1,3-二甲基苯含量显著增加,籽粒成熟过程中以积累芳香烃为主。在气味特征方面,随着籽粒的成熟,脂香强度明显增强,青香强度明显减弱。甜玉米品种之间存在差异,“仲甜9号”甜玉米成熟期时挥发性风味物质种类和含量明显高于其他2 个品种,且整体风味强度最大。     

A survey of lipolytic and glycolytic end-products in commercial Cheddar enzyme-modified cheese

The concentrations of L- and D-lactic acid and free fatty acids, C4:0 to C18:3, were quantified in a range of commercial enzyme-modified Cheddar cheeses. Lactic acid in Cheddar enzyme-modified cheeses varied markedly depending on the manufacturer. Differences in the ratio of L- to D-lactic acid indicate that cheeses of different age were used in their manufacture or contained varying levels of nonstarter lactic acid bacteria. The level of lipolysis in enzyme-modified cheese was higher than in natural Cheddar cheese; butyrate was the predominant free fatty acid. The addition of exogenous acetate, lactate, and butyrate was also indicated in some enzyme-modified cheeses and may be used to confer a specific flavor characteristic or reduce the pH of the product. Propionate was also found in some enzyme-modified cheese products and most likely originated from Swiss-type cheese used in their manufacture. Propionate is not normally associated with natural Cheddar cheese flavor; however, it may be important in the flavor and aroma of Cheddar enzyme-modified cheese. Levels of lipolysis and glycolysis appear to highly controlled as interbatch variability was generally low. Overall, the production of enzyme-modified Cheddar cheese involves manipulation of the end-products of glycolysis (lactate, propionate, and acetate) and lipolysis to generate products for specific applications.     

基于气相色谱-离子迁移谱法和固相微萃取-气相色谱-质谱法分析6种香型白酒挥发性风味物质

目的 比较6种香型白酒的挥发性风味物质差异。方法 采用气相色谱-离子迁移谱法(gas chromatography-ion mobility spectrometry, GC-IMS)和固相微萃取-气相色谱-质谱法(solid phase microextraction-gas chromatography-mass spectrometry, SPME-GC-MS)对6种不同香型白酒的挥发性成分进行分析, 结合气味活度值(odor activity value, OAV)确定其重要风味物质, 通过多元统计分析筛选差异香气成分。结果 GC-MS和GC-IMS分别在6种香型白酒中检测到56和77种化合物, 其中13种挥发性风味物质为2种技术共同检出; 挥发性成分主要是酯类、醇类和醛类; 不同白酒香气化合物含量差异较大, 如清香型白酒的乙酸乙酯含量显著高于其他白酒, 而己酸乙酯在浓香型白酒中含量最高; 通过偏最小二乘判别分析筛选出异戊醇、乙酸乙酯等18种挥发性风味物质作为区分不同白酒香气的差异化合物。结论 本研究采用两种技术协同分析, 获得6种香型白酒更全面的挥发性风味信息, 明确了6种香型白酒香气成分组成与差异, 为不同香型白酒风味调控奠定了基础。     

Quantification of volatile compounds in goat milk Jack cheese using static headspace gas chromatography

Goat milk Jack cheeses were manufactured with different levels of proteolytic endo- and exopeptidases from lysed bacterial cultures and aged for 30 wk. The aroma compounds that are potentially important in contributing the typical flavor of goat milk Jack cheese were quantified using static headspace gas chromatography. The concentrations of volatile compounds were evaluated every 6 wk throughout the aging period. Odor activity values of volatile compounds were calculated using the sensory threshold values reported in literature and their concentrations in Jack cheeses. Odor activity values of identified compounds were used to assess their potential contribution to the aroma of goat milk Jack cheeses. The odor activity values indicated that the ketones 2-hexanone, 2-heptanone, 2-nonanone, and 2,3-butanedione (diacetyl) were important odor-active compounds. The major odor-active acids found in this semi-hard goat milk cheese were butanoic, 2-methyl butanoic, pentanoic, hexanoic, and octanoic acids. Among the aldehydes, propanal and pentanal had high odor activity values and likely contributed to the aroma of this cheese. The concentrations of butanoic, pentanoic, hexanoic, heptanoic, octanoic, and nonanoic acids increased significantly in goat milk Jack cheese throughout aging. The extracted enzymes from lysed bacterial cultures that were added to the cheeses during manufacturing caused considerable increases in the concentrations of butanoic and hexanoic acids compared with the control. However, the lower concentration of peptidases resulted in an increased concentration of butanal, whereas more peptidases resulted in a lower concentration of 2-nonanone in goat milk Jack cheeses.     

Monitoring the ripening process of Cheddar cheese based on hydrophilic component profiling using gas chromatography-mass spectrometry

We proposed an application methodology that combines metabolic profiling with multiple appropriate multivariate analyses and verified it on the industrial scale of the ripening process of Cheddar cheese to make practical use of hydrophilic low-molecular-weight compound profiling using gas chromatography-mass spectrometry to design optimal conditions and quality monitoring of the cheese ripening process. Principal components analysis provided an overview of the effect of sodium chloride content and kind of lactic acid bacteria starter on the metabolic profile in the ripening process of Cheddar cheese and orthogonal partial least squares-discriminant analysis unveiled the difference in characteristic metabolites. When the sodium chloride contents were different (1.6 and 0.2%) but the same lactic acid bacteria starter was used, the 2 cheeses were classified by orthogonal partial least squares-discriminant analysis from their metabolic profiles, but were not given perfect discrimination. Not much difference existed in the metabolic profile between the 2 cheeses. Compounds including lactose, galactose, lactic acid, 4-aminobutyric acid, and phosphate were identified as contents that differed between the 2 cheeses. On the other hand, in the case of the same salt content of 1.6%, but different kinds of lactic acid bacteria starter, an excellent distinctive discrimination model was obtained, which showed that the difference of lactic acid bacteria starter caused an obvious difference in metabolic profiles. Compounds including lactic acid, lactose, urea, 4-aminobutyric acid, galactose, phosphate, proline, isoleucine, glycine, alanine, lysine, leucine, valine, and pyroglutamic acid were identified as contents that differed between the 2 cheeses. Then, a good sensory prediction model for “rich flavor,” which was defined as “thick and rich, including umami taste and soy sauce-like flavor,” was constructed based on the metabolic profile during ripening using partial least squares regression analysis. The amino acids proline, leucine, valine, isoleucine, pyroglutamic acid, alanine, glutamic acid, glycine, lysine, tyrosine, serine, phenylalanine, methionine, aspartic acid, and ornithine were extracted as ripening process markers. The present study is not limited to Cheddar cheese and can be applied to various maturation-type natural cheeses. This study provides the technical platform for designing optimal conditions and quality monitoring of the cheese ripening process.     

不同香型白酒感官风味及挥发性化合物结构特征

白酒的感官风味特性及其特征风味化合物组成是认识、判别白酒香型类别及鉴定白酒品质的重要基础，但目前关于不同香型白酒感官和风味化合物的研究尚不充分。本研究以酱香、浓香、清香和清酱香4 种香型白酒为研究对象，采用感官风味评价法结合顶空固相微萃取/液液微萃取-气相色谱-质谱联用法和气相色谱法-氢火焰离子化检测器分析技术对4 种香型白酒中的主要挥发性化合物进行分析，利用香气活度值筛选出特征挥发性化合物，并经偏最小二乘回归分析建立相关性评价模型。结果表明：4 种香型白酒的风味轮廓存在明显差异；所有样品中共含有251 种主要挥发性化合物，其中有54 种特征风味化合物；异戊酸乙酯、二甲基三硫醚、丁酸乙酯、糠醛、2,3,5-三甲基吡嗪和2,3,5,6-四甲基吡嗪对酱香型白酒风味贡献大；己酸乙酯、对甲酚和γ-壬内酯是浓香型白酒特征风味形成的关键化合物；壬醛、癸酸乙酯和苯乙醇是清香型白酒中特征性风味化合物；二甲基三硫醚、乙酸苯乙酯、苯乙醇、壬醛、癸醛、月桂酸乙酯和异戊醇则显著贡献了清酱香型白酒的特征风味。结论：本研究全面揭示并比较了不同香型白酒感官风味和化合物的多样性特征以及风味差异的表达机制，可为探索白酒风味特征的相关研究提供理论依据，并为后续研究白酒风味-健康机理提供参考。     

SPME/GC-MS Characterization and Comparison of Volatiles of Eleven Varieties of Turkish Cheeses

In this study, the volatile aroma profiles of a variety of economically important cheeses for the Turkish dairy sector were characterized. A total of 75 samples belonging to 11 Turkish cheese varieties, including Civil, Canak, Dil, Divle Tulum, Ezine, Hellim, Malatya, Mihalic, Orgu, Urfa, and Van Otlu, were comparatively studied for their volatile profiles. One hundred and twelve volatile compounds were identified in the cheeses by solid-phase microextraction combined with gas chromatography-mass spectrometry and the results are discussed based on their chemical classes (31 esters, 7 acids, 18 ketones, 3 aldehydes, 24 alcohols, 10 terpenes, and 19 miscellaneous compounds). Esters, ketones, and alcohols were the most abundant classes identified and were highly dependent on the variety of cheese. Principal component analysis was applied to aid the interpretation of the gas chromatography-mass spectrometry data and to distinguish the cheeses. Divle Tulum cheese had high levels of aldehydes, ketones, and alcohols and separated from all the other cheeses, and the cheeses including Dil, Hellim, Malatya, Orgu, and Urfa grouped together. The last group of cheeses had low levels of volatiles stemming probably from the restricting effect of scalding or cooking that are employed in the manufacture of these cheeses and on the biochemical and/or microbial activity. Civil, Ezine, and Mihalic cheeses had somewhat different aroma profiles, but they were closely located near the cheeses including Dil, Urfa, Orgu, etc. The results suggest that each variety of cheese had different volatiles profile and that the manufacturing technique as well as ripening conditions of the cheeses played a major role on the individual volatile profiles.     

Ripening of cheddar cheese with added attenuated adjunct cultures of lactobacilli

We made Milled curd Cheddar cheese with Lactococcus starter and an adjunct culture of Lactobacillus helveticus I or Lactobacillus casei T subjected to different attenuation treatments: freeze shocking (FS), heat shocking (HS), or spray drying (SD). Proteolysis during cheese ripening (0 to 6 mo), measured by urea-PAGE and water-soluble nitrogen, indicated only minor differences between control and most adjunct-treated cheeses. However, there were significant differences in the effect of Lactobacillus adjuncts on the level of free amino nitrogen in cheese. Cheeses made with FS or HS Lb. helveticus adjunct exhibited significantly greatest rates of free amino group formation. Lipolysis as measured by total free fatty acids was consistently highest in adjunct-treated cheeses, and FS Lb. casei-treated cheeses showed the highest rate of free fatty acid formation followed by FS Lb. helveticus treated cheeses. Mean flavor and aroma scores were significantly higher for cheeses made with Lb. helveticus strain. Freeze-shocked Lb. helveticus-treated cheeses obtained the highest flavor and aroma scores. Sensory evaluation indicated that most of the adjunct-treated cheeses promoted better texture and body quality.