酱鸭与香辛料风味物质及其在加工过程中的变化
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摘要
风味是肉制品的一个重要的质量指标,目前国内外对鸭肉的风味成分研究的很少。本文选取我国传统特色鸭肉制品酱鸭作为原料,研究了酱鸭挥发性风味物质的分析方法、酱鸭的特征风味物质、风味活性化合物对酱鸭风味贡献的大小以及加工工艺对鸭肉挥发性风味物质的影响。主要研究结果如下：
1、采用不同萃取技术研究了酱鸭的挥发性风味成分。以酱鸭为样品,以萃取时间、萃取温度、萃取样品量为因素对固相微萃取方法(SPME)进行优化选择。确定酱鸭挥发性风味成分的最佳萃取条件为：75μmCarb-PDMS萃取头,萃取温度为5O℃,萃取时间为45min,4g样品质量。比较了萃取溶剂和萃取时间对同时蒸馏萃取法(SDE)萃取效果的影响,结果显示乙醚比较适合作为SDE法萃取酱鸭挥发性风味成分的萃取剂,萃取时间为2h。综合两种方法,共鉴定出107种风味成分,固相微萃取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,两种方法可以相互较好地补充用于酱鸭挥发性风味分析。
2、利用SPME法和SDE法结合气相色谱-嗅闻仪-质谱(GC-O-MS)联用定性定量分析酱鸭特征风味化合物,共鉴定出35种酱鸭风味活性成分。SPME法鉴定出其中的27种,SDE鉴定出其中的22种。香味提取物稀释分析法(AEDA)鉴别酱鸭中的气味活性组分,定量测定各气味活性组分对酱鸭整体风味的贡献大小。化合物按对酱鸭整体风味贡献大小由高到低排序为：己醛、3-甲硫基丙醛、二甲基三硫化合物、壬醛、癸醛、反,反-2,4-壬二烯醛、反-2-癸烯醛、反,反-2,4-癸二烯醛、2-甲基丁醛、庚醛、2-甲基-3-呋喃硫醇、反,反-2,4-辛二烯醛、糠硫醇、1-辛烯-3-醇、反-2-壬烯醛、反-2-辛烯醛、1-戊烯-3-醇、乙酸乙酯、甲基硫醇、反-2-辛烯醛、2-戊基呋喃、苯甲醛。
3、采用超临界CO2萃取(SFE)对酱鸭的挥发性成分进行提取。经单因素和响应面优化得到的最佳萃取条件为：萃取压力11MPa、温度41℃、时间60min,在此条件下酱鸭挥发性成分的萃取比率为83.45%。SFE可以萃取出大部分酱鸭挥发性风味组分,萃取物的风味与原料非常接近。
4、桂皮、八角和小茴香对鸭肉挥发性影响较大,主要是茴香醛、桂皮醛和茴香脑加入鸭肉中较多。而白芷、草果和砂仁等香辛料对鸭肉的挥发性影响较小。腌制、烤制和煮制等加工工艺都可以使鸭肉的挥发性香味成分含量增加,氧化程度增加。与生鸭肉比较,烤制的鸭肉挥发性香味成分增加明显,其次是煮制鸭肉,最后是腌制鸭肉。脂质氧化降解、美拉德反应、氨基酸降解等反应产物构成了鸭肉的整体挥发性风味。
Flavor is one of the most important sensory properties of meat product. At present, few reports were about the volatile compounds of sauced duck meat. Sauced duck, the traditional Chinese duck product, was chosen to investigate the analysis method of sauced duck volatile flavor, the characteristic aroma compounds, the contribution of each odor-active component to the whole sauced duck flavor profile and the effect of process on the volatile flavor compounds. Main results are as follows:
1. Sauced duck aroma compounds were analyzed using different extraction techniques. The solid phase microextraction (SPME) analysis conditions such as the extraction time, temperature and sample quantity were optimized. The optimized conditions of SPME for aroma compounds extraction of sauced duck meat were that the 75μm CAR-PDMS fiber was exposed to the vapor phase above 4g sample for 45min at 50℃. The simultaneous distillation extraction (SDE) method was comparatively studied by using different extraction time and extraction solvents. The results indicated that ethyl ester was the preferable extraction solvent and extraction time is 2h.107 volatile flavor compounds were identified by two methods. SPME provided better extraction for volatiles having a lower boiling point, while SDE method was better for higher boiling point. As for analyzing the flavor compounds of sauced duck, SPME and SDE methods are of their own special benefits, and should be complementary by each other.
2.35 aroma active compounds were identified by SPME and SDE with GC-O-MS.27 aroma active were identified by SPME, while 22 by SDE. AEDA was used to quantify the contribution of each odor-active component to the whole sauced duck flavor profile. The order according to significance of the sauced duck aroma was hexanal; 3-(methylthio) propionaldehyde; dimethy trisulfide; nonanal; decanal; (E, E)-2,4-nonadienal; (E)-2-decenal; (E, E)-2,4-decadienal; 2-methyl-butanal; heptanal; 2-methyl-3-furanthiol; (E,E)-2,4-octadienal; furfuryl mercaptan; 1-octen-3-ol; (E)-2-nonenal; (E)-2-octenal; 1-penten-3-ol; acetic ether; methyl mercaptan; (E)-2-octenal; 2-pentyl furan; benzaldehyde.
3. The volatile components in sauced duck were extracted by supercritical-CO2 fluid. Single-factor and RSM were conducted for the optimum extraction parameters: extraction pressure 11MPa, extraction temperature 41℃, extraction period 1h. The extraction ratio of volatile components was 83.45% using optimized SC-CO2 extraction, and the extracts had high olfactory resemblance to the original sauced duck.
4. Cassia, aniseed and cumin had great effect on the volatiles of the duck, the most compounds the duck absorbed were anisic aldehyde, cinnamal and anethole. Ammi majus, amomi costati and amomi had less effect. Soused, grilled, cooking and other processing techniques can increase the volatile components and the degree of oxidation of duck meat. Compared with the raw duck, the largest increase of the volatile flavor components were roast duck, followed by cooking duck, while the least was soused duck. The overall volatile flavor composition of the duck meat was contributed by the products of lipid oxidation, Maillard reaction and amino acid degradation.
1、采用不同萃取技术研究了酱鸭的挥发性风味成分。以酱鸭为样品,以萃取时间、萃取温度、萃取样品量为因素对固相微萃取方法(SPME)进行优化选择。确定酱鸭挥发性风味成分的最佳萃取条件为：75μmCarb-PDMS萃取头,萃取温度为5O℃,萃取时间为45min,4g样品质量。比较了萃取溶剂和萃取时间对同时蒸馏萃取法(SDE)萃取效果的影响,结果显示乙醚比较适合作为SDE法萃取酱鸭挥发性风味成分的萃取剂,萃取时间为2h。综合两种方法,共鉴定出107种风味成分,固相微萃取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,两种方法可以相互较好地补充用于酱鸭挥发性风味分析。
2、利用SPME法和SDE法结合气相色谱-嗅闻仪-质谱(GC-O-MS)联用定性定量分析酱鸭特征风味化合物,共鉴定出35种酱鸭风味活性成分。SPME法鉴定出其中的27种,SDE鉴定出其中的22种。香味提取物稀释分析法(AEDA)鉴别酱鸭中的气味活性组分,定量测定各气味活性组分对酱鸭整体风味的贡献大小。化合物按对酱鸭整体风味贡献大小由高到低排序为：己醛、3-甲硫基丙醛、二甲基三硫化合物、壬醛、癸醛、反,反-2,4-壬二烯醛、反-2-癸烯醛、反,反-2,4-癸二烯醛、2-甲基丁醛、庚醛、2-甲基-3-呋喃硫醇、反,反-2,4-辛二烯醛、糠硫醇、1-辛烯-3-醇、反-2-壬烯醛、反-2-辛烯醛、1-戊烯-3-醇、乙酸乙酯、甲基硫醇、反-2-辛烯醛、2-戊基呋喃、苯甲醛。
3、采用超临界CO2萃取(SFE)对酱鸭的挥发性成分进行提取。经单因素和响应面优化得到的最佳萃取条件为：萃取压力11MPa、温度41℃、时间60min,在此条件下酱鸭挥发性成分的萃取比率为83.45%。SFE可以萃取出大部分酱鸭挥发性风味组分,萃取物的风味与原料非常接近。
4、桂皮、八角和小茴香对鸭肉挥发性影响较大,主要是茴香醛、桂皮醛和茴香脑加入鸭肉中较多。而白芷、草果和砂仁等香辛料对鸭肉的挥发性影响较小。腌制、烤制和煮制等加工工艺都可以使鸭肉的挥发性香味成分含量增加,氧化程度增加。与生鸭肉比较,烤制的鸭肉挥发性香味成分增加明显,其次是煮制鸭肉,最后是腌制鸭肉。脂质氧化降解、美拉德反应、氨基酸降解等反应产物构成了鸭肉的整体挥发性风味。
Flavor is one of the most important sensory properties of meat product. At present, few reports were about the volatile compounds of sauced duck meat. Sauced duck, the traditional Chinese duck product, was chosen to investigate the analysis method of sauced duck volatile flavor, the characteristic aroma compounds, the contribution of each odor-active component to the whole sauced duck flavor profile and the effect of process on the volatile flavor compounds. Main results are as follows:
1. Sauced duck aroma compounds were analyzed using different extraction techniques. The solid phase microextraction (SPME) analysis conditions such as the extraction time, temperature and sample quantity were optimized. The optimized conditions of SPME for aroma compounds extraction of sauced duck meat were that the 75μm CAR-PDMS fiber was exposed to the vapor phase above 4g sample for 45min at 50℃. The simultaneous distillation extraction (SDE) method was comparatively studied by using different extraction time and extraction solvents. The results indicated that ethyl ester was the preferable extraction solvent and extraction time is 2h.107 volatile flavor compounds were identified by two methods. SPME provided better extraction for volatiles having a lower boiling point, while SDE method was better for higher boiling point. As for analyzing the flavor compounds of sauced duck, SPME and SDE methods are of their own special benefits, and should be complementary by each other.
2.35 aroma active compounds were identified by SPME and SDE with GC-O-MS.27 aroma active were identified by SPME, while 22 by SDE. AEDA was used to quantify the contribution of each odor-active component to the whole sauced duck flavor profile. The order according to significance of the sauced duck aroma was hexanal; 3-(methylthio) propionaldehyde; dimethy trisulfide; nonanal; decanal; (E, E)-2,4-nonadienal; (E)-2-decenal; (E, E)-2,4-decadienal; 2-methyl-butanal; heptanal; 2-methyl-3-furanthiol; (E,E)-2,4-octadienal; furfuryl mercaptan; 1-octen-3-ol; (E)-2-nonenal; (E)-2-octenal; 1-penten-3-ol; acetic ether; methyl mercaptan; (E)-2-octenal; 2-pentyl furan; benzaldehyde.
3. The volatile components in sauced duck were extracted by supercritical-CO2 fluid. Single-factor and RSM were conducted for the optimum extraction parameters: extraction pressure 11MPa, extraction temperature 41℃, extraction period 1h. The extraction ratio of volatile components was 83.45% using optimized SC-CO2 extraction, and the extracts had high olfactory resemblance to the original sauced duck.
4. Cassia, aniseed and cumin had great effect on the volatiles of the duck, the most compounds the duck absorbed were anisic aldehyde, cinnamal and anethole. Ammi majus, amomi costati and amomi had less effect. Soused, grilled, cooking and other processing techniques can increase the volatile components and the degree of oxidation of duck meat. Compared with the raw duck, the largest increase of the volatile flavor components were roast duck, followed by cooking duck, while the least was soused duck. The overall volatile flavor composition of the duck meat was contributed by the products of lipid oxidation, Maillard reaction and amino acid degradation.
引文
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