采用同时蒸馏萃取-气相色谱/质谱分析小茴香的挥发性成分

通过比较精油收率及精油气相色谱分析含有的组分数量,确定同时蒸馏萃取方法提取小茴香挥发性成分较佳条件为乙醚萃取剂,小茴香∶乙醚∶水为10g∶40mL∶100mL,提取时间3h。气质联机分析所提取的挥发油,鉴定出反式茴香脑(7456%)、爱草脑(240%)、葑酮(105%)、茴香醛(351%)、1,8桉树脑(015%)、樟脑(005%)、萜烯类(297%)、香豆素(003%)、十八碳烯酸(018%)等43种化合物,总相对百分含量为8903%。     

沟槽滤嘴截留挥发性烟气成分的同时蒸馏萃取条件研究

为研究沟槽滤嘴对卷烟烟气中挥发性成分的截留情况,建立了同时蒸馏萃取-GC/MS分析的定性定量分析方法,并通过正交试验对同时蒸馏萃取条件进行了优化.结果表明,在抽吸烟支数量、GC/MS分析条件一定时,同时蒸馏萃取条件为:NaCl溶液浓度90 g/L,NaCl溶液用量400 mL,CH2Cl2用量40 mL,萃取时间2.5 h.在此条件下,从抽吸后沟槽滤嘴中分析出的挥发性烟气成分种类最多,总量最高.     

Physicochemical characteristics, textural properties and volatile compounds in comminuted sausages as affected by various fat levels and fat replacers

Physicochemical and textural properties, and volatile compounds of comminuted sausages with various added fat levels and fat replacers were evaluated. Sausages without added fat had higher expressible moisture and texture values, but their lightness and yellowness values were lower, as compared with sausages with 5%, 10%, or 15% fat. Increased fat levels with constant amounts of lean meat and added water increased the lightness and yellowness values, but tended the redness values tended to be similar. Low‐fat sausages (LFSs, <3%) containing non‐meat proteins, except egg white protein, had reduced texture values similar to those of regular‐fat counterparts (RFC). The addition of non‐meat proteins, except egg white protein, as components of fat replacers in LFS improved the textural characteristics, making them similar to those of RFC. LFSs containing sodium caseinate had reduced concentrations of pentadecanal and octadecanal, resulting in similar volatile compositions to those of RFC. Thus, sodium caseinate was the best non‐meat protein for the improvement of both texture and flavour of LFSs.     

不同产地香椿籽风味物质提取及成分分析

比较了从河南、湖北、陕西三地采集的香椿籽样品的挥发油含量和化学成分的差异。运用同步蒸馏萃取法提取香椿籽挥发油，所得挥发油通过GC／MS分析，并与Nist98标准图谱进行对照，定性分析了三种不同产地香椿籽挥发油，共鉴定出52种化学成分，三种挥发油均含有的主要成分是α波旁烯、γ-榄香烯、石竹烯及马兜铃烯。为香椿籽挥发油药用价值的进一步开发奠定了基础。     

Effect of pork fat addition on the volatile compounds of foal dry-cured sausage

The effect of fat content on volatile compounds from foal dry-cured sausage was studied. Three batches (10 units per batch) of dry fermented sausages with different pork back fat content (5%, 10% and 20%) were manufactured; low fat (LF), medium fat (MF) and high fat (HF), respectively. A total of 45 volatile compounds were extracted by purge-and-trap and identified by GC-MS in the headspace of the batches. The mixture comprised 11 terpenes, 15 esters, 14 hydrocarbons and 2 alcohols. Spices were responsible for the generation of 14 volatile compounds comprising terpenes and hydrocarbons. After 49 days of ripening volatile compounds from spices represented 52.9, 38.9 and 31.2% of the total area for samples from LF, MF and HF batches, respectively, while lipid autooxidation was responsible for the generation of 8 volatile compounds. The PCA offered a good separation of the mean samples according to their fat content.     

炖煮羊肉香气物质分析鉴定

本文对炖煮羊肉的香气物质进行了分析鉴定。采取的方法为先同时蒸馏萃取,萃取物再气相色谱-质谱联用及芳香提取物稀释法气相色谱-嗅闻分析。气相色谱-质谱联用分析,通过NIST2014质谱库检索和保留指数核对,共鉴定出142种挥发性成分,包括醛类、酮类、醇类、酯类、酸类、含硫化合物、含氮杂环、含氧杂环、烃类等,其中醛类所占比例最大。含量较高的为十六醛（18.82%）、壬醛（11.67%）、十八醛（4.75%）、己醛（2.54%）、辛醛（2.11%）等。芳香提取物稀释法气相色谱-嗅闻分析,结合气-质鉴定结果,将保留指数及气味特征与文献比对,鉴定出41种香气活性物质,其中3-（甲硫基）丙醛、糠硫醇、2-乙基-3,5-二甲基吡嗪、双（2-甲基-3-呋喃基）二硫醚、2,3-二甲基吡嗪、（Z）-2-壬烯醛、3-壬烯醛、12-甲基十三醛等14种化合物具有较高的稀释因子（log2FD≥7）,这些化合物被认为是关键香气成分。      

三桠苦叶挥发性成分的分析及在卷烟中的应用

以三桠苦的叶片为原料,采用常规提取法开发新型烟用香料。利用同时蒸馏萃取装置收集挥发性成分并用气相色谱-质谱仪进行分析和鉴定。并用峰面积归一化法确认了各种成分的相对含量,共鉴定出24种化合物。其主要成分为3,4,4α,5,6,8α-6H-2,5,5,8α-四甲基-2H-1-苯并吡喃(1.33%),2,6-二甲喹啉(2.49%),9-甲基-S-八氢蒽(0.95%),榄香素(0.55%),斯巴醇(0.67%),丁基化羟基甲苯(38.78%),2,4,6-三异丙基苯乙酮(2.16%),六乙苯(17.95%),邻苯二甲酸二丁酯(0.52%),2,4,6-三特丁基-苯酚(5.53%),植醇(0.71%)。并进行了卷烟加料试验,结果表明:该提取物具有增加烟气甜润感和细腻性、柔和烟气、提升烟气浓度和丰富性、谐调烟香的作用。     

A study of volatile flavour substances in Dalmatian traditional smoked ham: Impact of dry-curing and frying

Volatiles from Dalmatian prosciutto were isolated by solvent extraction (SE), simultaneous distillation extraction (SDE) and nitrogen purge and steam distillation (NPSD) and analyzed by GC and GC–MS. In all, 46 compounds were identified by SDE and SE (including fatty acids, aldehydes, phenols, esters, ketones and others), while 81 compounds were identified by NPSD (headspace volatiles including phenols, aldehydes, hydrocarbons, ketones, alcohols, esters and heterocyclic compounds). Regarding the impact of dry curing period on the volatiles, an increase in the percentages of aldehydes and esters during the ripening of the prosciutto was observed. Quantitative percentage differences among fried and raw samples were particularly evident in respect of aldehydes (SDE and SE). The NPSD method provided additional information of the volatiles from fried ham, since the pyrazines and most of the lower aldehydes that are important thermally derived flavour compounds were only isolated by NPSD (not by SE and SDE).     

吹扫捕集-气质联用法测定天然饮用水中挥发性有机物

采用吹扫捕集-气相色谱/质谱联用法,测定天然饮用水中35种挥发性有机化合物,包括三卤甲烷、卤代苯类、苯系物以及多环芳烃类等。方法检出限范围为0.05～0.17μg/L,35种有机物加标5μg/L测定回收率为86.5%～113%,RSD(n=6)为1.6%～6.1%。调研了市售的44个瓶装天然饮用水和5个水源水样品:瓶装天然饮用水中检出1,2-二氯乙烷、一氯二溴甲烷、二氯一溴甲烷、三溴甲烷、苯、三氯甲烷、1,2,4-三甲苯、甲苯共8个化合物,其中三氯甲烷的检出率达到49%,但检测结果均在相关标准的限量要求范围内;水源水样品中均未测得挥发性有机化合物。     

花生油炸制油条香气物质的分析鉴定

采取同时蒸馏萃取制备样品,气相色谱-质谱联用(GC-MS)、稀释法气相色谱-嗅闻(GC-O)对花生油炸制油条香气成分进行分析鉴定。基于检索NIST14质谱库、保留指数,气-质联机鉴定出83种化合物,包括醛类、酮类、醇类、酯类、酸类、含硫化合物、含氮杂环、含氧杂环、烃类、其他类,含量最高的是醛类,其中己醛、壬醛、(E)-2-癸烯醛、(E,Z)-2,4-癸二烯醛的含量远高于鉴定出的所有其它化合物。基于GC-MS鉴定结果、嗅闻的保留指数、嗅闻的气味特征及标准品,GC-O分析鉴定出30种香气活性物质,其中3-羟基-2-丁酮、3-乙基-2,5-二甲基吡嗪、糠醇、(E,E)-2,4-癸二烯醛、2,3-二甲基吡嗪、己醛、庚醛、(E)-2-壬烯醛、(E)-2-癸烯醛、(E)-2-十一烯醛、3-甲基丁醛、3-甲硫基丙醛、丙醛、辛醛、壬醛、(Z)-2-癸烯醛、1-辛烯-3-醇等17种化合物具有较高的稀释因子(log₂FD≥5)。通过本实验研究发现,花生油炸制油条中挥发性化合物种类丰富,构成了花生油条独特的油脂香、焦香、甜香等风味,其中醛类、含氧杂环化合物及含氮杂环化合物含量较高,是花生油炸制油条风味物质的主要成分。     

同时蒸馏萃取法提取新疆孜然精油的研究

研究以新疆孜然精油的最大提取率为目标,研究了同时蒸馏萃取孜然精油的提取工艺,分析了萃取时间、物料粒径、溶剂加入量对孜然精油提取率的影响,并通过正交试验得到了最佳的提取条件:萃取时间为1h,物料粒径为120目,溶剂加入量为80 mL.在此条件下孜然精油的萃取得率为2.71％.对同时蒸馏萃取孜然精油进行物理化学分析和GC-MS分析表明,同时蒸馏萃取新疆孜然精油工艺稳定可靠,具有极高的应用价值.     

The storage stability and textural, physico-chemical and sensory quality of low-fat ground pork patties with Carrageenan as fat replacer

Low‐fat ground pork patties (<10% total fat) made with carrageenan added at either 0.25, 0.50 or 0.75% final concentration were processed and the compositional and sensory characteristics compared with control patties which contained 20% fat. The moisture content of raw and cooked low‐fat patties was significantly (P < 0.05) higher than control patties because of greater amounts of water added during formulation. Cooking yield, fat and moisture retention also improved significantly (P < 0.05) in low‐fat patties that had carrageenan incorporated when compared to a control product. The dimensions of the low‐fat patties were maintained better than those of the control product during cooking. The sensory attributes of low‐fat patties with 0.5% carrageenan were similar to those of the high‐fat control. The lipid profile revealed as much as a 47.7 or 44.1% decrease in total lipids and cholesterol content respectively, compared with the controls. The calorie content was reduced by 31.1% in low‐fat cooked patties compared with the controls. The texture profile of low‐fat patties that had been made with 0.5% carrageenan were similar to control patties with only a slight increase in hardness and gumminess in the low‐fat product. The low‐fat ground pork patties made in the present study remained stable without any appreciable loss of physico‐chemical, microbiological and organoleptic quality during refrigerated storage (4 ± 1 °C) for 21 and 35 days in aerobic and vacuum packaging respectively.     

Effect of the inclusion of chestnut in the finishing diet on volatile compounds during the manufacture of dry-cured “Lacón” from Celta pig breed

The effect of the finishing diet on the volatile compounds throughout the manufacture of dry-cured “lacón” (a Spanish traditional meat product), from the Celta pig breed was studied. Thirty-six pigs were separated into three groups according to the type of feeding during the finish-fattening period of three months (concentrate, mixed diet and chestnut). From the pigs of each diet, four batches of dry-cured “lacón” were manufactured. From each batch, samples of fresh meat, meat after salting, after post-salting, and after 14, 28, 56 and 84 days of drying–ripening were taken. Volatiles were extracted by a purge-and-trap method and analyzed by gas chromatographic/mass spectrometry (GC/MS). Seventy-six volatile compounds were identified and quantified from dry-cured “lacón” samples in pigs finished with chestnut, eighty-two for concentrate fed pigs and eighty in pigs fed with the mixed diet. The number of identified volatile compounds increased during the manufacturing process; at 84 days of drying–ripening, in the dry-cured “lacón” samples from pigs finished with concentrate, mixed diet and chestnut, 54, 58 and 62 volatile compounds were detected, respectively. The most abundant group of flavour compounds at the end of the manufacturing process was hydrocarbons in the three feeding systems, followed by aldehydes, ketones and alcohols. Discriminant analysis selected six variables (dodecane, butadienol, pentenol, 2-pentenal, decen-3-ona and pyridine-2-methyl) and calculated two discriminating functions which allowed verification of chestnut in the finishing diet.     

罐罐肉加工与贮藏过程中挥发性物质变化的研究

为了探明雅安罐罐肉挥发性物质的变化规律,本研究以不同加工与贮藏阶段的罐罐肉为对象,用同时蒸馏萃取结合气相色谱/质谱法对挥发性化合物进行分析。结果显示,罐罐肉在加工与贮藏过程中共检测出120种挥发性物质,醇、醛、酮、烃、酰胺、酯是主要成分,其中以己醛和2,4-癸二烯醛为主的醛类物质相对含量最高（最高达64.42%）。在加工过程中醛、酮、酯显著增加,并检测出酰胺类物质。在贮藏过程中醇、醛、酮的相对含量整体呈现下降趋势,烃类、酰胺类、酯类和其他化合物的相对含量整体呈上升趋势,并新产生了（2E）-2-十一碳烯醛、甲酸己酯、（Z）-9-十八烯酸酰胺和2-戊基呋喃等物质。      

一种萃取酒醅中低沸点挥发性成分的方法

分别采用水蒸汽蒸馏（SD）法、超声辅助溶剂萃取（UASE）法和蒸馏-微溶剂萃取（SD-MSE）法从浓香型白酒酒醅中提取挥发性成分,利用峰面积归一化法测定各成分的相对含量,通过对挥发性成分的气相色谱-质谱连用/自动化退卷积系统（GC-MS/AMDIS）对比分析。结果表明,SD、UASE及SD-MSE法分别鉴定出42种、71种、60种挥发性成分。SD、UASE及SD-MSE法分别测得的醇、酸、酯的相对含量分别为1.34%、6.61%、21.67%;1.03%、39.28%、37.42%;3.96%、9.97%、64.97%。由此可知,SD法对酸、酯的提取效果劣于另两种方法,UASE法对酸类物质萃取效果更佳,SD-MSE法对酯类物质的萃取效果更佳。和UASE法相比,SD-MSE法节约了大量溶剂,减少了样品转移次数,且待测液澄清透明,是一种适宜萃取糟醅中低沸点成分的方法。     

SDE-GC-MS与P&T-TD-GC-MS提取分析不同香型凤凰单丛茶香气比较

分别采用同时蒸馏萃取(simultaneous distillation extraction,SDE)法和吹扫捕集热脱附解吸(purge and trap thermal desorption,PT-TD)法提取黄栀香和肉桂香两种香型凤凰单丛茶的香气成分并用气相色谱-质谱进行分析比较。结果表明,2种方法提取的香气成分和相对含量比例有很大差异,两者各有优劣,相互补充,结合分析更加完整,更有利于准确地进行香型分类,并发现PT-TD法有更大的运用空间。SDE法提取的萜烯类化合物较多,脂肪族和芳香族的化合物较少,不同香型的区别主要是成分的相对含量比例;PT-TD法提取得到的成分种类多,不同香型的茶区别较大。通过萜酯指数可得PT-TD法提取的香气更为清香,SDE法提取的香气较为浓烈,但两者都体现了凤凰茶清高持久的幽香特性。SDE法的高温加热可能引起成分的改变,PT-TD提取法的成分较能真实地反应茶汤冲泡的特点。结合2种方法分析得出,黄栀香与肉桂香茶的区别明显,黄栀香茶以荜澄茄醇、橙花叔醇等为主,并特有丙酸芳樟酯、δ-杜松烯、萜品油烯等成分;肉桂香茶是吲哚、δ-壬内酯、苯乙腈相对含量多,且含有苯乙醇、苯甲醇、1,5,8-对-薄荷三烯、戊醛等特有成分。     

The profile in polyphenols and volatile compounds in alcoholic beverages from different cultivars of mulberry

Abstract: Mulberry fruits have different chemical compositions because of cultivar variation. In this study, polyphenol profile and volatile composition of alcoholic beverages produced from different mulberries of Da 10, Hongguo 2 hao, and Hongguo 1 hao were investigated. Statistically significant differences were detected in the chemical composition of the analyzed alcoholic beverage samples. The beverage of Da 10 possessed the highest content of total phenols, total flavonoids, and total anthocyanins, which was determined by spectrophotometry analysis, contrarily Hongguo 1 hao beverage showing the lowest. Phenolic acids and flavonols were analyzed by high performance liquid chromatography analysis. Protocatechuic acid was the main phenolic acid in all analyzed alcoholic beverage samples, and its concentration ranged from 8.20 mg L^?1 (Hongguo 1 hao beverage) to 29.98 mg L^?1 (Da 10 beverage). High level of flavonols was found in both Da 10 and Hongguo 2 hao beverage samples, whereas Hongguo 1 hao beverage sample was characterized with lower level of flavonols. Furthermore, volatile compounds were analyzed by solid phase microextraction‐gas chromatography mass spectrometry analysis. The amount of esters varied widely among the 3 alcoholic beverage samples. The concentration of aliphatic alcohols in Hongguo 2 hao and 1 hao beverage samples was higher than Da 10 sample, whereas Da 10 beverage sample contained more aromatic alcohols than the others. Hongguo 1 beverage sample showed the highest concentration of acetic acid. This study demonstrated that quantitative differences of phenolic compounds and volatile compounds among cultivars were significant, which highly affected the quality of alcoholic beverage from mulberry. Practical Application: Mulberry fruits had different chemical compositions because of cultivar variation. The analyzed Da 10 cultivar of mulberry appeared to be a good raw material for alcoholic beverage‐making because of its high level of total sugar and acidity. This study demonstrated that alcoholic beverages from mulberry contain high amounts of polyphenols. These bioactive compounds may act synergistically to promote health, and reduce risk factors of chronic diseases.     

香菇精的提取与成分分析

先确定了香菇水蒸汽蒸馏所得总挥发性物质——香菇精的相对含量分析方法，然后通过多个单因素试验确定的香菇精水蒸气蒸馏的优化提取工艺条件为：50g原料粉碎至100目，按1：15固液比加入2L圆底烧瓶中，水蒸气蒸馏提取2h。再结合气质联用仪分析，对优化工艺条件下香菇精馏分中的成分进行分析，检测出包括主要呈味物质在内的13种化合物。