鸭肉风味及其在加工过程中的变化研究
摘要
风味是肉品最重要的食用品质之一，目前国内外对鸭肉风味的研究很少，尤其是对我国传统特色鸭肉制品盐水鸭风味的研究还是空白。本课题是国家863项目“中国传统及特色食品和畜产品生产技术与产品开发”(2002AA248031)以及江苏省十五科技攻关项目“传统特色肉制品现代加工、保鲜技术及其标准化研究”(BE2001400)”的一部分，目的是研究鸭肉风味以及加工对风味形成的作用，探索鸭肉风味形成的机理和途径，为鸭肉产品传统工艺的现代化改造提供理论依据。具体研究内容和结果如下：
1．鸭肉挥发性风味分析方法研究
采用不同萃取技术研究了鸭肉的挥发性香气成分。以南京盐水鸭胸肉为样品，以萃取时间、萃取温度、萃取样品量、萃取头为因素对固相微萃取方法进行了优化选择。确定鸭肉挥发性风味成分固相微萃取方法的最佳分析条件为：75μmCarb-PDMS萃取头，4g样品质量，萃取温度为45℃，40min萃取时间。采用不同萃取剂比较了同时蒸馏萃取(SDE)方法，结果显示乙醚是鸭肉挥发性风味成分的较好的萃取剂。采用顶空固相微萃取、吹扫捕集-热脱附(PT-TD)以及同时蒸馏萃取三种萃取技术提取盐水鸭香气，并用气质联用(GC-MS)进行分析，通过比较质谱以及卡瓦茨保留指数(KI)鉴定香气成分。共鉴定出116种化合物，包括醛类(31种)、酯类(4种)、醇类(14种)、酸类(7种)、烃类(25种)、酮类(15种)、呋喃类(7种)以及含N化合物(5种)、含S化合物(8种)。固相微萃取和吹扫捕集-热脱附方法对低沸点化合物萃取效果较好，而同时蒸馏萃取法对高沸点化合物萃取效果较好。固相微萃取方法优于吹扫捕集-热脱附法，而固相微萃取和同时蒸馏萃取两种方法可以相互较好补充用于鸭肉挥发性风味分析。
2．鸭肉主体特征香味成分研究
采用不同萃取时间同时蒸馏萃取研究吲哚在鸭肉中的来源，结果显示在15min-1h同时蒸馏萃取液中没有检测到吲哚，而只在2h及其以后的萃取液中检测到了吲哚，且吲哚的含量随着时间是呈指数增加的(R~2=0.9989)。吲哚不是鸭肉本身的成分，而是在预处理即同时蒸馏萃取时生成的后续反应产物。将同时蒸馏萃取液按pH值进行分离，中性组分和碱性组分构成鸭肉的主体特征风味。采用固相微萃取比较分析了鸭胸和尾部的肉和脂肪的挥发性成分，在尾部鸭肉中检测到的支链脂肪酸2-甲基己酸、4-甲基己酸、4-甲基辛酸，是首次在禽肉中鉴定出的。以不同部位鸭肉样品采用固相微萃取和同时蒸馏萃取气相嗅觉分析方法鉴定出鸭肉主体特征成分为：甲硫醇、2-甲基丙醛、3-甲基丁醛、3-羟基-2-丁酮、二甲基二硫、2-甲基噻吩、2-甲基-3-呋喃硫醇、3-甲硫基丙醛、(Z)-2-庚烯醛、二甲基三硫、1-辛烯-3-醇、4-甲基己酸、2-乙酰基噻唑、(E，E)-2，4-壬二烯醛、4-甲基辛酸、(E，E)-2，4-癸二烯醛。此外以下16种化合物也对鸭肉的整体风味有较大贡献：1-戊烯-3-醇、2，3-戊二酮、己醛、甲基吡嗪、糠醛、2-呋喃甲醇、(E)-2-己烯醛、丁基内酯、2-辛酮、2．戊基呋喃、乙酸己酯、(E)-2-辛烯醛、壬醛、2-甲酰噻吩、(E)-2-壬烯醛、(E)-2-癸烯醛。
3．加工对鸭肉风味前体物及滋味成分的作用
盐水鸭加工过程中，水分含量具有下降的趋势，蛋白质和脂肪含量持续增加。干腌加工使得还原糖、硫胺素以及单不饱和脂肪酸和多不饱和脂肪酸含量显著减少(p＜0.05)；复卤加工中重要的风味前体物质没有显著变化；烘烤加工的鸭肉还原糖含量显著下降(p＜0.05)，而硫胺素含量没有变化，但游离脂肪酸含量增加；煮制加工中硫胺素、还原糖以及游离脂肪酸含量显著下降(p＜0.05)。对于磷脂脂肪酸，煮制前的加工过程中磷脂脂肪酸几乎没有变化，而煮制过程中含量下降。盐水鸭煮制前的加工中，各种游离氨基酸以及游离氨基酸总量随着加工进程都有不同程度的增加，尤其是复卤和烘烤过程；煮制为成品后，盐水鸭中所有的游离氨基酸含量剧减(p＜0.05)，大部分氨基酸减少了50％以上。盐水鸭加工过程中大部分小肽含量具有减少的趋势，但复卤加工中大多数肽类和肽类总量比干腌鸭肉显著增加(P＜0.05)。风味核苷酸5′-IMP和5′-GMP在煮制前的加工中持续减少，煮制过程中大量增加(P＜0.05)
不同加工鸭肉水分含量以及pH值差异显著(P＜0.05)。盐水鸭pH最低；烤鸭的水分含量最高，而脂肪含量最低；水煮鸭的水份含量最低，脂肪含量及pH值最高。不同加工鸭肉产品的还原糖含量差异不显著(p＞0.05)，而硫胺素含量差异显著(p＜0.05)。水煮鸭的硫胺素含量最低，烤鸭次之，而盐水鸭含量最高。不同加工鸭肉产品游离脂肪酸含量的差异主要表现在多不饱和脂肪酸，烤鸭的多不饱和脂肪酸含量最低，盐水鸭和水煮鸭没有差异。大多数磷脂脂肪酸盐水鸭含量最低，而烤鸭和水煮鸭差异不大。就大多数游离氨基酸和肽类而言，盐水鸭和烤鸭的含量没有显著差异，且高于水煮鸭的含量。盐水鸭的总游离氨基酸含量最高，而烤鸭和水煮鸭的含量差异不显著(p＞0.05)。盐水鸭中所有核苷酸含量都显著高于水煮鸭(P＜0.05)。烤鸭的风味核苷酸含量最高，其次为盐水鸭，水煮鸭含量最少。
除复卤加工外，其他加工均对风味前体物质有一定影响。三种加工方式对还原糖参加的风味反应没有显著差异；硫胺素降解对盐水鸭的风味作用较小，而对烤鸭和水煮鸭有一定的作用。盐水鸭较低的pH值和适于食用的食盐含量，对其鲜味的感官特性影响较大。盐水鸭加工过程中复卤工艺对鸭肉滋味成分作用显著。盐水鸭特殊的加工工艺使得盐水鸭具有较高的脂质氧化降解、鲜味氨基酸Asp、Glu和甜味氨基酸Ala含量、小肽含量以及风味核苷酸5′-IMP和5′-GMP含量是其美味的原因所在。
4．加工对鸭肉挥发性风味的作用
采用顶空固相微萃取技术分析了盐水鸭加工过程中挥发性风味成分的变化，并比较了盐水鸭、烤鸭、水煮鸭三种鸭肉产品的香气成分。在盐水鸭加工过程中共有92种化合物被鉴定出来，其中有57种是首次在鸭肉中鉴定出来的。这些化合物包括醇类(13种)、醛类(22种)、烃类(25种)、酸类(4种)、酮类(12种)、酯类(5种)、呋喃类(3种)、含硫化合物(6种)、含氮化合物(2种)。在盐水鸭加工中，干腌使得鸭肉氧化程度增加，部分特征香味成分含量增加，而复卤和烘烤作用不大，煮制使得鸭肉香味成分急剧增加同时氧化值升高。主成分分析显示，第一主成分(PCI)解释了97％的变异，包括戊醛、己醛、辛醛、壬醛和2，3-辛二酮，来源于脂肪氧化和降解。三种不同加工鸭肉产品在挥发性成分上的差异主要是含量上，而不是种类上。除了酯类化合物，水煮鸭其余种类的化合物含量均低于烤鸭和盐水鸭。与盐水鸭相比，烤鸭在烃类、酯类和酮类化合物的含量上较低，而在醇类、醛类和含硫含氮化合物上含量较高。脂质氧化降解是形成鸭肉特征风味的必要条件，美拉德反应对于鸭肉熟肉香味起决定性的作用，而脂质-美拉德反应相互作用对鸭肉整体香味构成具有重要的作用。
5．脂质对鸭肉风味贡献研究
采用石油醚以及氯仿甲醇有选择的除去鸭肉中的甘油三酯和磷脂，对去脂肉进行感官评定和仪器分析。感官评定分析表明去除磷脂和甘油三酯的鸭肉感官特性主要为烘烤的、坚果的气味，而鸭的特征气味以及肉香得分则很低，与对照组以及仅去除甘油三酯的鸭肉差异极显著(p＜0.01)。两者的挥发性成分差异很大，前者主要是烃类、酸类以及酯类化合物，没有鸭肉特征香味成分，且其他重要的香味活性成分含量也均显著低于后者。甘油三酯对鸭肉的特征性风味以及肉香影响不大，而磷脂则作用巨大。通过对比氯仿甲醇萃取的脂质以及其水洗后的脂质挥发性成分发现对照鸭脂特征香味成分的含量均显著高于水洗鸭脂(p＜0.05)，且在水洗鸭脂中没有鉴定出含硫含氮化合物。感官特性表明鸭脂质中的水溶性成分对鸭肉肉香有显著贡献，而对鸭种属风味特性没有贡献。未氧化鸭脂种属气味感官得分极显著低于氧化的鸭脂(p＜0.01)，具有较高的甜玉米的气味得分。经过氧化的鸭脂氧化腐败感官得分显著高于仅热处理的鸭脂。感官评定表明脂质氧化显著贡献于鸭的种属特征风味。在未氧化的鸭脂中醛类、酮类化合物较少，没有鉴定出2-戊基呋喃，但二甲硫含量显著高于氧化鸭脂(P＜0.05)。经过氧化的鸭脂其鸭肉特征性成分及其他香味活性成分含量均显著高于未氧化的样品(P＜0.05)。
Flavor is one of the most important sensory property of meat and meat product. However, little reports on the volatile compounds or taste compounds of duck meat were presented, especially no reports was on the flavor of traditional Chinese duck meat product—Nanjing water-boiled salted duck. This research is a part of the items entitled "Producing technology and products exploitation for Chinese traditional & character food and animal products"(2002AA248031) under the high technology and development program of P. R. China and "Modern process, preservative technique and standardization of traditional Chinese feature meat product"(BE2001400) under the science and technology tackle key problem program of Jiangsu province. The aim is to investigate the duck flavor and effects of process on the duck meat flavor and provide a theory basis in improving the processing technology and realizing the industrial production of duck meat product. The contents and results are as follows.1. Studies on the analysis method of duck volatile flavor compoundsDuck aroma compounds were analyzed using different extraction techniques. The solid phase microextraction (SPME) analysis conditions were optimized, which the extraction time, temperature, sample quality and fibers were optimize by using water-boiled salted duck breast meat. The optimized conditions of spme for analysis of duck meat were that a 75μm carboxen-polydimethylsiloxane (CAR-PDMS) SPME fiber was exposed to the vapor phase above 7 g sample for 40 min at 45℃. The simultaneous distillation extraction (SDE) method was comparatively studied by using three different extraction solvents. Result indicated that ethyl ester was the preferable extraction solvent. Three extraction techniques including SPME, purge and trap with thermal desorption (PT-TD) and SDE were comparatively used to extract the aroma compounds of duck. The extracted aroma was then analyzed by gas chromatography-mass spectrometry (GC-MS). Total 116 volatile flavor compounds were identified by comparing the mass spectrometry and Kràtz retention index (KI), which aldehydes (31 kinds), esters (4 kinds), alcohols (14 kinds), acids (7 kinds), hydrocarbons (25 kinds), kentons (15 kinds), N-containing compounds (5 kinds), S-containing compounds (8 kinds)and furans (7 kinds) were included. SPME and PT-TD method provided better extraction for volatiles having a lower molecular mass, while the results of SDE method was inverse. As for analyzing the flavor compounds of duck meat, SPME method was better than PT-TD method and SPME with SDE method may well complement each other.
2. Studies on the characteristic aroma compounds of duck
Simultaneous distillation extraction (SDE) by different extraction time was used to analyze the origin of indole. Result indicated that indole was detected only in the extract that the extraction time long than 2h, and the content of indole rose exponentially (R~2=0.9989) with the increasing extraction time. It is obvious that indole was not the genuine substance in the duck, but that it was formed during the extraction of the volatiles from duck meat. SDE extract was separated by pH value and then were analyzed, which found the neutural fraction and the basic fraction could be the important component of duck meat aroma. Different part of duck meat and fat including duck breast and duck caudal were analyzed using solid phase microextraction (SPME). The branch fatty acids including 2-methyl hexanoic acid, 4-methyl hexanoic acid and 4-methyl octanoic acid, were identified in the duck caudal meat and fat. These branch fatty acids were the first identified in poultry meat, which could contribute the typical flavor of duck. The SPME-GC-O and SDE-GC-O were used in the different part of duck meat and fat to identify the principal characteristic compounds of duck meat, and a total 16 compounds were identified as follows: methanethiol, 2-methyl propanal, 3-methyl butanal, 3-hydroxy-2-butanone, dimethyl disulfide, 2-methyl thiophene, 2-methyl-3-furanthiol, 3-(methylthio)-propanal, (Z)-2-heptenal, dimethyl trisulfide, 1-octen-3-ol, 4-methyl hexanoic acid, 2-acetyl-thiazole, (E,E)-2,4-nonadienal, 4-methyl octanoic acid, (E,E)-2,4-decadienal. The following sixteen compounds were contributed to the overall flavor of duck: 1-penten-3-ol, 2,3-pentanedione, hexanal, methylpyrazine, furfural, 2-furanmethanol, (E)-2-hexenal, butyrolactone, 2-octanone, 2-pentyl furan, acetic acid hexyl ester, (E)-2-octenal, nonanal, 2-formylthiophene, (E)-2-nonenal, (E)-2-decenal.
3. Studies oneffect of process on duck flavor precursor and taste compounds
During the processing of Nanjing water-boiled salted duck, the content of water of duck has a decrease tendency during the processing, while the protein and fat content increased continuously. The, thiamine, MUFA and PUFA content decreased during the dry-curing (p＜0.05). No significant changes of the important flavor precursor happened during the brining. During the roasting, the reducing sugar decreased significantly and the thiamine didn't change, while the free fatty acids increased. As for phospholipids fatty acid, no changed was found before the process of boiling. The important precursor compounds decreased significantly during the boiling. Before the boiling of the processing of NJWSD, all kinds of FAA and total FAA increased in different degree, especially for the processing of brining and roasting. During the boiling, all the FAA decreased (p＜0.05), most of them decreased to 50%. Most of small peptide content had a decreasing tendency, while most small peptide and the total peptide increased in brined duck than those of in dry-cured duck (p＜0.05). The flavor nucleotides 5'-IMP and 5'-GMP continuously decreased before the process of boiling, but largely increased during the boiling.
The significant differences were observed in moisture and pH value of different processed duck meat product, which the NJWSD was in the lowest pH value, and roasted duck were in the highest content of moisture and lowest fat content. As for water-boiled duck, the fat content and pH value were the highest. No significant difference between three different processed duck products in reducing sugar content was observed. But the content of thiamine of three different processed duck products differed significantly, which the contend of thiamine in water-boiled duck was the lowest, followed was the roasted duck and the content in NJWSD was the highest, he main difference among different processed duck meat was on the PUFA, which the roasted duck possessed the lowest level of PUFA. As for phospholipids, the PFA of water-boiled salted was the highest among three different processed duck, while roasted duck and water-boiled duck had no difference. The content of most FAA and peptides, no difference was observed between NJWSD and roasted duck, and higher than those of in water-boiled duck. The total of FAA in NJWSD was the highest, while the roasted duck and water-boiled duck were in the same level. All the nucleotides in NJWSD were higher than that of in water-boiled duck. The content of flavor nucleotides in roasted duck was the highest among three different processed duck, followed was the NJWSD and the water-boiled salted duck.
Except the brining process, else process during the processing of NJWSD had an effect on the content of flavor precursor. No difference between three process styles were observed in the effect on the flavor reaction by reducing sugar. Among three processed duck, the decomposition degree of thiamine in water-boiled salted duck was the least, while that of in roasted duck and water-boiled duck were higher. The lower pH value and suitable content of salt of water-boiled salted duck were largely contributed to the umami sensory property. The brining process in water-boiled salted duck had great effect on the taste compounds of duck meat. The higher oxidation and decomposition degree of fat, highercontent of umami amino acids asp and glu, sweet amino acid ala, small peptides and flavor nucleotides 5'-IMP and 5'-GMP were the reason of delicious for the water-boiled salted duck and roasted duck, which was one of the reasons constituting the delicious of water-boiled salted duck.
4. Studies on the effect of process on the duck volatile flavor compounds
Changes in volatile flavor compounds during the processing of water-boiled salted duck were investigated using solid phase microextraction, and three processed duck meat product including water-boiled salted duck, roasted duck and water-boiled duck were compared for their aroma compounds, to study the effect of process on the duck aroma and discuss the mechanism of the formation of duck meat volatile flavor compounds. Total 92 compounds were identified during the processing water-boiled salted duck, which 57 compounds were detected firstly in duck meat. These compounds included alcohols (13 kinds), aldehydes (22kinds), hydrocarbons (25 kinds), acids (4kinds), ketones (12 kinds), esters (5 kinds), furans (3 kinds), N-containing compounds (2 compounds) and S-containing compounds (6 kinds). During the processing of water-boiled salted duck, dry-curing accelerated the oxidation and increased the formation of some characteristic aroma compounds, but the effect of brining and roasting were little. The boiling process made the duck aroma compounds level sharp and high the oxidation value. The first principal component (PC1) explained 97% of the total variance of the data, in which pentanal, hexanal, octanal, nonanal, and 2,3-octanedione were the main compounds. Three different processed duck products were not different in kinds of volatiles, but were the content, of that. Except esters, other kinds of compounds in water-boiled duck were lower than those of water-boiled salted duck and roasted duck. Compared to the water-boiled salted duck, roasted duck were higher in alcohols, aldehydes, N-and S-containing compounds, but lower in hydrocarbons, esters, ketones. Lipid oxidation and decomposition were the necessary condition for the formation characteristic aroma of duck, and Maillard reaction was decisive to the cooked duck meat aroma. Interactions between compounds produced by the reaction of intermediates of the Maillard reaction with lipid oxidation products importantly influence the overall aroma profiles of cooked duck meat.
5. Studies on the effect of duck fat on the duck odour
Duck fat was extracted selectively using petroleum spirit and chloroform with methanol respectively. Sensory analysis and instrument analysis showed that the duck meat sensory property were roasted and nutty when the phospholipids and triglycerides were removed, while the duck characteristic aroma score were significantly low (p＜0.01) compared to the petroleum spirit test. The volatile compounds differed greatly, which the former contained the hydrocarbons, acids and esters mainly, and no duck characteristic aroma compounds were found in the former sample. The other important active aroma compounds were also significantly lower than the later. Triglycerides had little effect on the duck characteristic and meaty aroma, but phospholipid was.
Duck fat extracted by chloroform with methanol was washed by water to remove the water soluble compounds in fat. No S- and N- containing compounds were identified in washed duck fat, and the characteristic aroma compounds were significantly lower (p＜0.01) than the control duck fat. The water soluble compounds in duck fat contributed the duck meaty aroma but not the characteristic aroma of duck.
Non-oxidative duck fat with a higher corn score, had a significantly lower score in duck odour than that of oxidative duck fat (p＜0.01). The oxidative duck fat had a higher score in oxidation and rancid than that of non-oxidative duck fat (p＜0.01). Little aldehydes and ketones was identified in non-oxidative duck fat, and no 2-pentyl furan was found also. But dimethyl sulfide was higher(P＜0.05) in non-oxidative duck fat than that of oxidative duck fat. Fat oxidation significantly contributed to the duck odour. The duck characteristic aroma compounds and other active aroma compounds in oxidative duck fat were higher(P＜0.05) than those of in non-oxidative duck fat.
1．鸭肉挥发性风味分析方法研究
采用不同萃取技术研究了鸭肉的挥发性香气成分。以南京盐水鸭胸肉为样品，以萃取时间、萃取温度、萃取样品量、萃取头为因素对固相微萃取方法进行了优化选择。确定鸭肉挥发性风味成分固相微萃取方法的最佳分析条件为：75μmCarb-PDMS萃取头，4g样品质量，萃取温度为45℃，40min萃取时间。采用不同萃取剂比较了同时蒸馏萃取(SDE)方法，结果显示乙醚是鸭肉挥发性风味成分的较好的萃取剂。采用顶空固相微萃取、吹扫捕集-热脱附(PT-TD)以及同时蒸馏萃取三种萃取技术提取盐水鸭香气，并用气质联用(GC-MS)进行分析，通过比较质谱以及卡瓦茨保留指数(KI)鉴定香气成分。共鉴定出116种化合物，包括醛类(31种)、酯类(4种)、醇类(14种)、酸类(7种)、烃类(25种)、酮类(15种)、呋喃类(7种)以及含N化合物(5种)、含S化合物(8种)。固相微萃取和吹扫捕集-热脱附方法对低沸点化合物萃取效果较好，而同时蒸馏萃取法对高沸点化合物萃取效果较好。固相微萃取方法优于吹扫捕集-热脱附法，而固相微萃取和同时蒸馏萃取两种方法可以相互较好补充用于鸭肉挥发性风味分析。
2．鸭肉主体特征香味成分研究
采用不同萃取时间同时蒸馏萃取研究吲哚在鸭肉中的来源，结果显示在15min-1h同时蒸馏萃取液中没有检测到吲哚，而只在2h及其以后的萃取液中检测到了吲哚，且吲哚的含量随着时间是呈指数增加的(R~2=0.9989)。吲哚不是鸭肉本身的成分，而是在预处理即同时蒸馏萃取时生成的后续反应产物。将同时蒸馏萃取液按pH值进行分离，中性组分和碱性组分构成鸭肉的主体特征风味。采用固相微萃取比较分析了鸭胸和尾部的肉和脂肪的挥发性成分，在尾部鸭肉中检测到的支链脂肪酸2-甲基己酸、4-甲基己酸、4-甲基辛酸，是首次在禽肉中鉴定出的。以不同部位鸭肉样品采用固相微萃取和同时蒸馏萃取气相嗅觉分析方法鉴定出鸭肉主体特征成分为：甲硫醇、2-甲基丙醛、3-甲基丁醛、3-羟基-2-丁酮、二甲基二硫、2-甲基噻吩、2-甲基-3-呋喃硫醇、3-甲硫基丙醛、(Z)-2-庚烯醛、二甲基三硫、1-辛烯-3-醇、4-甲基己酸、2-乙酰基噻唑、(E，E)-2，4-壬二烯醛、4-甲基辛酸、(E，E)-2，4-癸二烯醛。此外以下16种化合物也对鸭肉的整体风味有较大贡献：1-戊烯-3-醇、2，3-戊二酮、己醛、甲基吡嗪、糠醛、2-呋喃甲醇、(E)-2-己烯醛、丁基内酯、2-辛酮、2．戊基呋喃、乙酸己酯、(E)-2-辛烯醛、壬醛、2-甲酰噻吩、(E)-2-壬烯醛、(E)-2-癸烯醛。
3．加工对鸭肉风味前体物及滋味成分的作用
盐水鸭加工过程中，水分含量具有下降的趋势，蛋白质和脂肪含量持续增加。干腌加工使得还原糖、硫胺素以及单不饱和脂肪酸和多不饱和脂肪酸含量显著减少(p＜0.05)；复卤加工中重要的风味前体物质没有显著变化；烘烤加工的鸭肉还原糖含量显著下降(p＜0.05)，而硫胺素含量没有变化，但游离脂肪酸含量增加；煮制加工中硫胺素、还原糖以及游离脂肪酸含量显著下降(p＜0.05)。对于磷脂脂肪酸，煮制前的加工过程中磷脂脂肪酸几乎没有变化，而煮制过程中含量下降。盐水鸭煮制前的加工中，各种游离氨基酸以及游离氨基酸总量随着加工进程都有不同程度的增加，尤其是复卤和烘烤过程；煮制为成品后，盐水鸭中所有的游离氨基酸含量剧减(p＜0.05)，大部分氨基酸减少了50％以上。盐水鸭加工过程中大部分小肽含量具有减少的趋势，但复卤加工中大多数肽类和肽类总量比干腌鸭肉显著增加(P＜0.05)。风味核苷酸5′-IMP和5′-GMP在煮制前的加工中持续减少，煮制过程中大量增加(P＜0.05)
不同加工鸭肉水分含量以及pH值差异显著(P＜0.05)。盐水鸭pH最低；烤鸭的水分含量最高，而脂肪含量最低；水煮鸭的水份含量最低，脂肪含量及pH值最高。不同加工鸭肉产品的还原糖含量差异不显著(p＞0.05)，而硫胺素含量差异显著(p＜0.05)。水煮鸭的硫胺素含量最低，烤鸭次之，而盐水鸭含量最高。不同加工鸭肉产品游离脂肪酸含量的差异主要表现在多不饱和脂肪酸，烤鸭的多不饱和脂肪酸含量最低，盐水鸭和水煮鸭没有差异。大多数磷脂脂肪酸盐水鸭含量最低，而烤鸭和水煮鸭差异不大。就大多数游离氨基酸和肽类而言，盐水鸭和烤鸭的含量没有显著差异，且高于水煮鸭的含量。盐水鸭的总游离氨基酸含量最高，而烤鸭和水煮鸭的含量差异不显著(p＞0.05)。盐水鸭中所有核苷酸含量都显著高于水煮鸭(P＜0.05)。烤鸭的风味核苷酸含量最高，其次为盐水鸭，水煮鸭含量最少。
除复卤加工外，其他加工均对风味前体物质有一定影响。三种加工方式对还原糖参加的风味反应没有显著差异；硫胺素降解对盐水鸭的风味作用较小，而对烤鸭和水煮鸭有一定的作用。盐水鸭较低的pH值和适于食用的食盐含量，对其鲜味的感官特性影响较大。盐水鸭加工过程中复卤工艺对鸭肉滋味成分作用显著。盐水鸭特殊的加工工艺使得盐水鸭具有较高的脂质氧化降解、鲜味氨基酸Asp、Glu和甜味氨基酸Ala含量、小肽含量以及风味核苷酸5′-IMP和5′-GMP含量是其美味的原因所在。
4．加工对鸭肉挥发性风味的作用
采用顶空固相微萃取技术分析了盐水鸭加工过程中挥发性风味成分的变化，并比较了盐水鸭、烤鸭、水煮鸭三种鸭肉产品的香气成分。在盐水鸭加工过程中共有92种化合物被鉴定出来，其中有57种是首次在鸭肉中鉴定出来的。这些化合物包括醇类(13种)、醛类(22种)、烃类(25种)、酸类(4种)、酮类(12种)、酯类(5种)、呋喃类(3种)、含硫化合物(6种)、含氮化合物(2种)。在盐水鸭加工中，干腌使得鸭肉氧化程度增加，部分特征香味成分含量增加，而复卤和烘烤作用不大，煮制使得鸭肉香味成分急剧增加同时氧化值升高。主成分分析显示，第一主成分(PCI)解释了97％的变异，包括戊醛、己醛、辛醛、壬醛和2，3-辛二酮，来源于脂肪氧化和降解。三种不同加工鸭肉产品在挥发性成分上的差异主要是含量上，而不是种类上。除了酯类化合物，水煮鸭其余种类的化合物含量均低于烤鸭和盐水鸭。与盐水鸭相比，烤鸭在烃类、酯类和酮类化合物的含量上较低，而在醇类、醛类和含硫含氮化合物上含量较高。脂质氧化降解是形成鸭肉特征风味的必要条件，美拉德反应对于鸭肉熟肉香味起决定性的作用，而脂质-美拉德反应相互作用对鸭肉整体香味构成具有重要的作用。
5．脂质对鸭肉风味贡献研究
采用石油醚以及氯仿甲醇有选择的除去鸭肉中的甘油三酯和磷脂，对去脂肉进行感官评定和仪器分析。感官评定分析表明去除磷脂和甘油三酯的鸭肉感官特性主要为烘烤的、坚果的气味，而鸭的特征气味以及肉香得分则很低，与对照组以及仅去除甘油三酯的鸭肉差异极显著(p＜0.01)。两者的挥发性成分差异很大，前者主要是烃类、酸类以及酯类化合物，没有鸭肉特征香味成分，且其他重要的香味活性成分含量也均显著低于后者。甘油三酯对鸭肉的特征性风味以及肉香影响不大，而磷脂则作用巨大。通过对比氯仿甲醇萃取的脂质以及其水洗后的脂质挥发性成分发现对照鸭脂特征香味成分的含量均显著高于水洗鸭脂(p＜0.05)，且在水洗鸭脂中没有鉴定出含硫含氮化合物。感官特性表明鸭脂质中的水溶性成分对鸭肉肉香有显著贡献，而对鸭种属风味特性没有贡献。未氧化鸭脂种属气味感官得分极显著低于氧化的鸭脂(p＜0.01)，具有较高的甜玉米的气味得分。经过氧化的鸭脂氧化腐败感官得分显著高于仅热处理的鸭脂。感官评定表明脂质氧化显著贡献于鸭的种属特征风味。在未氧化的鸭脂中醛类、酮类化合物较少，没有鉴定出2-戊基呋喃，但二甲硫含量显著高于氧化鸭脂(P＜0.05)。经过氧化的鸭脂其鸭肉特征性成分及其他香味活性成分含量均显著高于未氧化的样品(P＜0.05)。
Flavor is one of the most important sensory property of meat and meat product. However, little reports on the volatile compounds or taste compounds of duck meat were presented, especially no reports was on the flavor of traditional Chinese duck meat product—Nanjing water-boiled salted duck. This research is a part of the items entitled "Producing technology and products exploitation for Chinese traditional & character food and animal products"(2002AA248031) under the high technology and development program of P. R. China and "Modern process, preservative technique and standardization of traditional Chinese feature meat product"(BE2001400) under the science and technology tackle key problem program of Jiangsu province. The aim is to investigate the duck flavor and effects of process on the duck meat flavor and provide a theory basis in improving the processing technology and realizing the industrial production of duck meat product. The contents and results are as follows.1. Studies on the analysis method of duck volatile flavor compoundsDuck aroma compounds were analyzed using different extraction techniques. The solid phase microextraction (SPME) analysis conditions were optimized, which the extraction time, temperature, sample quality and fibers were optimize by using water-boiled salted duck breast meat. The optimized conditions of spme for analysis of duck meat were that a 75μm carboxen-polydimethylsiloxane (CAR-PDMS) SPME fiber was exposed to the vapor phase above 7 g sample for 40 min at 45℃. The simultaneous distillation extraction (SDE) method was comparatively studied by using three different extraction solvents. Result indicated that ethyl ester was the preferable extraction solvent. Three extraction techniques including SPME, purge and trap with thermal desorption (PT-TD) and SDE were comparatively used to extract the aroma compounds of duck. The extracted aroma was then analyzed by gas chromatography-mass spectrometry (GC-MS). Total 116 volatile flavor compounds were identified by comparing the mass spectrometry and Kràtz retention index (KI), which aldehydes (31 kinds), esters (4 kinds), alcohols (14 kinds), acids (7 kinds), hydrocarbons (25 kinds), kentons (15 kinds), N-containing compounds (5 kinds), S-containing compounds (8 kinds)and furans (7 kinds) were included. SPME and PT-TD method provided better extraction for volatiles having a lower molecular mass, while the results of SDE method was inverse. As for analyzing the flavor compounds of duck meat, SPME method was better than PT-TD method and SPME with SDE method may well complement each other.
2. Studies on the characteristic aroma compounds of duck
Simultaneous distillation extraction (SDE) by different extraction time was used to analyze the origin of indole. Result indicated that indole was detected only in the extract that the extraction time long than 2h, and the content of indole rose exponentially (R~2=0.9989) with the increasing extraction time. It is obvious that indole was not the genuine substance in the duck, but that it was formed during the extraction of the volatiles from duck meat. SDE extract was separated by pH value and then were analyzed, which found the neutural fraction and the basic fraction could be the important component of duck meat aroma. Different part of duck meat and fat including duck breast and duck caudal were analyzed using solid phase microextraction (SPME). The branch fatty acids including 2-methyl hexanoic acid, 4-methyl hexanoic acid and 4-methyl octanoic acid, were identified in the duck caudal meat and fat. These branch fatty acids were the first identified in poultry meat, which could contribute the typical flavor of duck. The SPME-GC-O and SDE-GC-O were used in the different part of duck meat and fat to identify the principal characteristic compounds of duck meat, and a total 16 compounds were identified as follows: methanethiol, 2-methyl propanal, 3-methyl butanal, 3-hydroxy-2-butanone, dimethyl disulfide, 2-methyl thiophene, 2-methyl-3-furanthiol, 3-(methylthio)-propanal, (Z)-2-heptenal, dimethyl trisulfide, 1-octen-3-ol, 4-methyl hexanoic acid, 2-acetyl-thiazole, (E,E)-2,4-nonadienal, 4-methyl octanoic acid, (E,E)-2,4-decadienal. The following sixteen compounds were contributed to the overall flavor of duck: 1-penten-3-ol, 2,3-pentanedione, hexanal, methylpyrazine, furfural, 2-furanmethanol, (E)-2-hexenal, butyrolactone, 2-octanone, 2-pentyl furan, acetic acid hexyl ester, (E)-2-octenal, nonanal, 2-formylthiophene, (E)-2-nonenal, (E)-2-decenal.
3. Studies oneffect of process on duck flavor precursor and taste compounds
During the processing of Nanjing water-boiled salted duck, the content of water of duck has a decrease tendency during the processing, while the protein and fat content increased continuously. The, thiamine, MUFA and PUFA content decreased during the dry-curing (p＜0.05). No significant changes of the important flavor precursor happened during the brining. During the roasting, the reducing sugar decreased significantly and the thiamine didn't change, while the free fatty acids increased. As for phospholipids fatty acid, no changed was found before the process of boiling. The important precursor compounds decreased significantly during the boiling. Before the boiling of the processing of NJWSD, all kinds of FAA and total FAA increased in different degree, especially for the processing of brining and roasting. During the boiling, all the FAA decreased (p＜0.05), most of them decreased to 50%. Most of small peptide content had a decreasing tendency, while most small peptide and the total peptide increased in brined duck than those of in dry-cured duck (p＜0.05). The flavor nucleotides 5'-IMP and 5'-GMP continuously decreased before the process of boiling, but largely increased during the boiling.
The significant differences were observed in moisture and pH value of different processed duck meat product, which the NJWSD was in the lowest pH value, and roasted duck were in the highest content of moisture and lowest fat content. As for water-boiled duck, the fat content and pH value were the highest. No significant difference between three different processed duck products in reducing sugar content was observed. But the content of thiamine of three different processed duck products differed significantly, which the contend of thiamine in water-boiled duck was the lowest, followed was the roasted duck and the content in NJWSD was the highest, he main difference among different processed duck meat was on the PUFA, which the roasted duck possessed the lowest level of PUFA. As for phospholipids, the PFA of water-boiled salted was the highest among three different processed duck, while roasted duck and water-boiled duck had no difference. The content of most FAA and peptides, no difference was observed between NJWSD and roasted duck, and higher than those of in water-boiled duck. The total of FAA in NJWSD was the highest, while the roasted duck and water-boiled duck were in the same level. All the nucleotides in NJWSD were higher than that of in water-boiled duck. The content of flavor nucleotides in roasted duck was the highest among three different processed duck, followed was the NJWSD and the water-boiled salted duck.
Except the brining process, else process during the processing of NJWSD had an effect on the content of flavor precursor. No difference between three process styles were observed in the effect on the flavor reaction by reducing sugar. Among three processed duck, the decomposition degree of thiamine in water-boiled salted duck was the least, while that of in roasted duck and water-boiled duck were higher. The lower pH value and suitable content of salt of water-boiled salted duck were largely contributed to the umami sensory property. The brining process in water-boiled salted duck had great effect on the taste compounds of duck meat. The higher oxidation and decomposition degree of fat, highercontent of umami amino acids asp and glu, sweet amino acid ala, small peptides and flavor nucleotides 5'-IMP and 5'-GMP were the reason of delicious for the water-boiled salted duck and roasted duck, which was one of the reasons constituting the delicious of water-boiled salted duck.
4. Studies on the effect of process on the duck volatile flavor compounds
Changes in volatile flavor compounds during the processing of water-boiled salted duck were investigated using solid phase microextraction, and three processed duck meat product including water-boiled salted duck, roasted duck and water-boiled duck were compared for their aroma compounds, to study the effect of process on the duck aroma and discuss the mechanism of the formation of duck meat volatile flavor compounds. Total 92 compounds were identified during the processing water-boiled salted duck, which 57 compounds were detected firstly in duck meat. These compounds included alcohols (13 kinds), aldehydes (22kinds), hydrocarbons (25 kinds), acids (4kinds), ketones (12 kinds), esters (5 kinds), furans (3 kinds), N-containing compounds (2 compounds) and S-containing compounds (6 kinds). During the processing of water-boiled salted duck, dry-curing accelerated the oxidation and increased the formation of some characteristic aroma compounds, but the effect of brining and roasting were little. The boiling process made the duck aroma compounds level sharp and high the oxidation value. The first principal component (PC1) explained 97% of the total variance of the data, in which pentanal, hexanal, octanal, nonanal, and 2,3-octanedione were the main compounds. Three different processed duck products were not different in kinds of volatiles, but were the content, of that. Except esters, other kinds of compounds in water-boiled duck were lower than those of water-boiled salted duck and roasted duck. Compared to the water-boiled salted duck, roasted duck were higher in alcohols, aldehydes, N-and S-containing compounds, but lower in hydrocarbons, esters, ketones. Lipid oxidation and decomposition were the necessary condition for the formation characteristic aroma of duck, and Maillard reaction was decisive to the cooked duck meat aroma. Interactions between compounds produced by the reaction of intermediates of the Maillard reaction with lipid oxidation products importantly influence the overall aroma profiles of cooked duck meat.
5. Studies on the effect of duck fat on the duck odour
Duck fat was extracted selectively using petroleum spirit and chloroform with methanol respectively. Sensory analysis and instrument analysis showed that the duck meat sensory property were roasted and nutty when the phospholipids and triglycerides were removed, while the duck characteristic aroma score were significantly low (p＜0.01) compared to the petroleum spirit test. The volatile compounds differed greatly, which the former contained the hydrocarbons, acids and esters mainly, and no duck characteristic aroma compounds were found in the former sample. The other important active aroma compounds were also significantly lower than the later. Triglycerides had little effect on the duck characteristic and meaty aroma, but phospholipid was.
Duck fat extracted by chloroform with methanol was washed by water to remove the water soluble compounds in fat. No S- and N- containing compounds were identified in washed duck fat, and the characteristic aroma compounds were significantly lower (p＜0.01) than the control duck fat. The water soluble compounds in duck fat contributed the duck meaty aroma but not the characteristic aroma of duck.
Non-oxidative duck fat with a higher corn score, had a significantly lower score in duck odour than that of oxidative duck fat (p＜0.01). The oxidative duck fat had a higher score in oxidation and rancid than that of non-oxidative duck fat (p＜0.01). Little aldehydes and ketones was identified in non-oxidative duck fat, and no 2-pentyl furan was found also. But dimethyl sulfide was higher(P＜0.05) in non-oxidative duck fat than that of oxidative duck fat. Fat oxidation significantly contributed to the duck odour. The duck characteristic aroma compounds and other active aroma compounds in oxidative duck fat were higher(P＜0.05) than those of in non-oxidative duck fat.
引文
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