南京板鸭肌内磷脂的分析检测及其在加工过程中的变化规律研究
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摘要
以南京板鸭原料及各工艺阶段产品为材料，探讨了南京板鸭肌内磷脂的组成、分子种和脂肪酸组成分析检测方法，并且研究了磷脂在板鸭加工过程中及原料加热过程中的变化规律。
1．建立了固相萃取净化和高效液相色谱法测定板鸭中几种肌内磷脂的方法。板鸭肌肉中的磷脂用氨丙基硅胶固相萃取柱纯化，然后用高效液相色谱正相柱分离。通过紫外检测器和蒸发光散射检测器串联检测显示，该测定方法回收率为81.0％～99.0％，相对标准偏差为1.5％～2.3％。将该法应用于板鸭样品的分析获得了较好的效果，经测定板鸭肌内脑磷脂(PE)、卵磷脂(PC)、磷脂酰丝氨酸(PS)、神经鞘磷脂(SPH)和溶血磷脂酰胆碱(LPC)分别占肌内脂肪的8.79％、14.67％、0.11％、0.52％和0.27％。
2．研究了南京板鸭在加工过程中各个工艺阶段的腿肌肌内磷脂与游离脂肪酸的变化情况。肌内脂质使用氯仿-甲醇溶液提取，采用固相萃取法将游离脂肪酸和磷脂与其他脂类分离，用高效液相色谱分析各种磷脂的含量，通过毛细管气相色谱分析了游离脂肪酸的含量。通过分析不同工艺阶段的样品，发现在南京板鸭加工过程中，各种磷脂显著减少，游离脂肪酸含量显著增加，游离脂肪酸的增加与磷脂的减少关系密切，特别是与脑磷脂的减少更为密切。
3．采用固相萃取提取鸭肉肌内磷脂，用高效液相色谱法在正相半制备硅胶柱上将PC、PE与其它成分分离，从柱后收集PC和PE，然后在反相C_(18)柱上分析其分子种组成，通过质谱对PC和PE的分子种进行鉴定，结合对其脂肪酸组成的气相色谱(GC)分析，得到主要分子种的结构。结果表明：在鸭肉肌内PC中含有C_(20∶4)／C_(16∶0) PC，C_(18∶1)／C_(16∶0) PC，C_(18∶2)／C_(18∶0) PC，C_(18∶2)／C_(16∶0) PC和C_(18∶1)／C_(18∶0) PC等5种主要分子种，5种PC的总含量为PC总量的92.05％；PE中含有C_(14∶0)／C_(22∶4) PE，C_(18∶0)／C_(20∶4) PE，C_(18∶0)／C_(18∶2) PE，C_(14∶1)／C_(24∶2) PE和C_(18∶1)／C_(18∶2) PE等5种主要分子种，5种PE的总含量为PE总量的92.48％。
4．进一步研究了鸭肉经过煮制和烘烤后肌内磷脂的变化情况。肌内脂质使用氯仿-甲醇溶液提取，采用固相萃取法将磷脂与其他脂类分离，用高效液相色谱分析各种
Green duck and each processing stages of Nanjing dry-cured ducks were as material, analysis and determination methods of composition, molecular species, fatty acids in phospholipids of Nanjing dry-cured duck muscle were discussed, and changing rules of dry-cured duck processing and green duck heating were studied.
1. A method of solid phase extraction (SPE) and high performance liquid chromatography (HPLC) for the determination of phospholipids in Nanjing dry-cured duck muscle was established. The phospholipids from dry-cured duck muscle were depurated by LRC-NH_2 SPE. Then the phospholipids were separated through NP-HPLC, and detected with the UV detector and ELSD, which were installed in series. The recovery was 81.0%-99.0%, and relative standard deviations were 1.5%-2.3%. This method was successfully used in the analysis of dry-cured duck sample, the proportion of phosphatidylethanolamine, phosphatidylcholine, phosphatidylserine, sphingomyelin and lysophosphatidylcholine in muscle fat were 8.79%,14.67%, 0.11%, 0.52% and 0.27% respectively.
2. Nanjing dry-cured duck was analyzed by studying the changes of phospholipids and free fatty acids in intramuscular lipids from crura muscle. Intramuscular lipids were distilled using chloroform and methanol, phospholipids and free fatty acids were separated by solid phase extraction (SPE), phospholipids were analyzed by HPLC, free fatty acids were determined via capillary gas chromatography. Through analyzing samples of each processing phase, the result displayed phospholipids were prominence decrease and free fatty acids were notability increase during processing of Nanjing dry-cured duck, the relation between increasing of free fatty acids and decreasing of phospholipids was tightness, especially the decreasing of phosphatidylcholine.
3. Intramuscular phospholipids was eluted by SPE, PC and PE was separated from duck muscle phospholipids on a normal phase semi-preparative silica gel column using HPLC, then collected from the column outlet, compositions of their molecular species were analyzed using a reverse phase C_(18) column, then the molecular species be identified by
1．建立了固相萃取净化和高效液相色谱法测定板鸭中几种肌内磷脂的方法。板鸭肌肉中的磷脂用氨丙基硅胶固相萃取柱纯化，然后用高效液相色谱正相柱分离。通过紫外检测器和蒸发光散射检测器串联检测显示，该测定方法回收率为81.0％～99.0％，相对标准偏差为1.5％～2.3％。将该法应用于板鸭样品的分析获得了较好的效果，经测定板鸭肌内脑磷脂(PE)、卵磷脂(PC)、磷脂酰丝氨酸(PS)、神经鞘磷脂(SPH)和溶血磷脂酰胆碱(LPC)分别占肌内脂肪的8.79％、14.67％、0.11％、0.52％和0.27％。
2．研究了南京板鸭在加工过程中各个工艺阶段的腿肌肌内磷脂与游离脂肪酸的变化情况。肌内脂质使用氯仿-甲醇溶液提取，采用固相萃取法将游离脂肪酸和磷脂与其他脂类分离，用高效液相色谱分析各种磷脂的含量，通过毛细管气相色谱分析了游离脂肪酸的含量。通过分析不同工艺阶段的样品，发现在南京板鸭加工过程中，各种磷脂显著减少，游离脂肪酸含量显著增加，游离脂肪酸的增加与磷脂的减少关系密切，特别是与脑磷脂的减少更为密切。
3．采用固相萃取提取鸭肉肌内磷脂，用高效液相色谱法在正相半制备硅胶柱上将PC、PE与其它成分分离，从柱后收集PC和PE，然后在反相C_(18)柱上分析其分子种组成，通过质谱对PC和PE的分子种进行鉴定，结合对其脂肪酸组成的气相色谱(GC)分析，得到主要分子种的结构。结果表明：在鸭肉肌内PC中含有C_(20∶4)／C_(16∶0) PC，C_(18∶1)／C_(16∶0) PC，C_(18∶2)／C_(18∶0) PC，C_(18∶2)／C_(16∶0) PC和C_(18∶1)／C_(18∶0) PC等5种主要分子种，5种PC的总含量为PC总量的92.05％；PE中含有C_(14∶0)／C_(22∶4) PE，C_(18∶0)／C_(20∶4) PE，C_(18∶0)／C_(18∶2) PE，C_(14∶1)／C_(24∶2) PE和C_(18∶1)／C_(18∶2) PE等5种主要分子种，5种PE的总含量为PE总量的92.48％。
4．进一步研究了鸭肉经过煮制和烘烤后肌内磷脂的变化情况。肌内脂质使用氯仿-甲醇溶液提取，采用固相萃取法将磷脂与其他脂类分离，用高效液相色谱分析各种
Green duck and each processing stages of Nanjing dry-cured ducks were as material, analysis and determination methods of composition, molecular species, fatty acids in phospholipids of Nanjing dry-cured duck muscle were discussed, and changing rules of dry-cured duck processing and green duck heating were studied.
1. A method of solid phase extraction (SPE) and high performance liquid chromatography (HPLC) for the determination of phospholipids in Nanjing dry-cured duck muscle was established. The phospholipids from dry-cured duck muscle were depurated by LRC-NH_2 SPE. Then the phospholipids were separated through NP-HPLC, and detected with the UV detector and ELSD, which were installed in series. The recovery was 81.0%-99.0%, and relative standard deviations were 1.5%-2.3%. This method was successfully used in the analysis of dry-cured duck sample, the proportion of phosphatidylethanolamine, phosphatidylcholine, phosphatidylserine, sphingomyelin and lysophosphatidylcholine in muscle fat were 8.79%,14.67%, 0.11%, 0.52% and 0.27% respectively.
2. Nanjing dry-cured duck was analyzed by studying the changes of phospholipids and free fatty acids in intramuscular lipids from crura muscle. Intramuscular lipids were distilled using chloroform and methanol, phospholipids and free fatty acids were separated by solid phase extraction (SPE), phospholipids were analyzed by HPLC, free fatty acids were determined via capillary gas chromatography. Through analyzing samples of each processing phase, the result displayed phospholipids were prominence decrease and free fatty acids were notability increase during processing of Nanjing dry-cured duck, the relation between increasing of free fatty acids and decreasing of phospholipids was tightness, especially the decreasing of phosphatidylcholine.
3. Intramuscular phospholipids was eluted by SPE, PC and PE was separated from duck muscle phospholipids on a normal phase semi-preparative silica gel column using HPLC, then collected from the column outlet, compositions of their molecular species were analyzed using a reverse phase C_(18) column, then the molecular species be identified by
引文
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1．卢行芳，卢荣．天然磷脂产品的加工及应用[M]．北京：化学工业出版社，2004．160-172．
2．赵改名，周光宏，徐幸莲，等．金华火腿加工过程中二肽酰肽酶Ⅰ的活性变化[J]．南京农业大学学报，2005，28(1)：94～98．
3．夏海涛，侯近龙，刘玉芬．高效液相色谱法分析大豆中磷脂酰胆碱的分子种[J]．分析试验室，2003，22(1)：9～11．
4. Folch J, Lees M, Stanley G H S. A silmple method for isolation and purification of total lipids from animal tissues [J]. Journal of Biology Chemistry, 1957, 226: 487～509.
5. García R J A, Gibert J, Díaz I. Determination of neutral lipids from subcutaneous fat of cured ham by capillary gas chromatography and liquid chromatography [J]. Journal of Chromatography A, 1994, 667: 225～233.
6. Lesnefsky J E, Stoll S K M. Separation and quantitation of phospholipids and lysophospholipids by high-performance liquid chromatography[J]. Analytical Biochemistry, 2002, 285: 246～254.
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1．卢行芳，卢荣．天然磷脂产品的加工及应用[M]．北京：化学工业出版社，2004．160～172．
2．杨红菊，乔发东，马长伟等．脂肪氧化和美拉德反应与肉品风味质量的关系[J]．肉类研究，2004，1：25～28．
3．夏海涛，侯近龙，刘玉芬．高效液相色谱法分析大豆中磷脂酰胆碱的分子种[J]．分析试验室，2003，22(1)：9～11．
4. Folch J, Lees M, Stanley G H S. A silmple method for isolation and purification of total lipids from animal tissues [J]. Journal of Biology Chemistry, 1957, 226: 487～509.
5. García R J A, Gibert J, Díaz I. Determination of neutral lipids from subcutaneous fat of cured ham by capillary gas chromatography and liquid chromatography [J]. Journal of Chromatography A, 1994, 667: 225～233.
6. Marco M, Fabio B, Emanuele B. Normal phase liquid chromatography-electrospray ionization tandem mass spectrometry analysis of phospholipid molecular species in blood mononuclear cells: application to cystic fibrosis[J]. Journal of Chromatography B, 2004, 810, 173～186
7. Lesnefsky J E, Stoll S K M. Separation and quantitation of phospholipids and lysophospholipids by high-performance liquid chromatography[J]. Analytical Biochemistry, 2002, 285: 246～254.
8. Yang H J, Ma C W, Qiao F D. Lipolysis in intramuscular lipids during processing of traditional Xuanwei ham [J]. Meat Science, 2005, 71, 670～675.
9. Gary D, Nigel D. Analysis of phospholipid molecular species by liquid chromatography atmospheric pressure chemical ionisation mass spectrometry of diacylglycerol nicotinates[J]. Chemistry and Physics of Lipids, 2001, 111, 1～17.
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11. Giorgis I, Dan B, Jan M. Analysis of phosphatidylcholine and sphingomyelin molecular species from brain extracts using capillary liquid chromatography electrospray ionization mass spectrometry[J]. Journal of Neuroscience Methods, 2003, 128, 111～119.
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1．卢行芳，卢荣．天然磷脂产品的加工及应用[M]．北京：化学工业出版社，2004．160～172．
2．杨红菊，乔发东，马长伟等．脂肪氧化和美拉德反应与肉品风味质量的关系[J]．肉类研究，2004，1：25～28．
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5. García R J A, Gibert J, Díaz I. Determination of neutral lipids from subcutaneous fat of cured ham by capillary gas chromatography and liquid chromatography [J]. Journal of Chromatography A, 1994, 667: 225～233.
6. Marco M, Fabio B, Emanuele B. Normal phase liquid chromatography-electrospray ionization tandem mass spectrometry analysis of phospholipid molecular species in blood mononuclear cells: application to cystic fibrosis[J]. Journal of Chromatography B, 2004, 810, 173～186
7. Lesnefsky J E, Stoll S K M. Separation and quantitation of phospholipids and lysophospholipids by high-performance liquid chromatography[J]. Analytical Biochemistry, 2002, 285: 246～254.
8. Yang H J, Ma C W, Qiao F D. Lipolysis in intramuscular lipids during processing of traditional Xuanwei ham [J]. Meat Science, 2005, 71, 670～675.
9. Gary D, Nigel D. Analysis of phospholipid molecular species by liquid chromatography atmospheric pressure chemical ionisation mass spectrometry of diacylglycerol nicotinates[J]. Chemistry and Physics of Lipids, 2001, 111, 1～17.
10. Begona B, Rainer B. LC-MS analysis of phospholipids and lysophospholipids in human bronchoalveolar lavage fluid[J]. Journal of Chromatography B, 2005, 814, 21～28.
11. Giorgis I, Dan B, Jan M. Analysis of phosphatidylcholine and sphingomyelin molecular species from brain extracts using capillary liquid chromatography electrospray ionization mass spectrometry[J]. Journal of Neuroscience Methods, 2003, 128, 111～119.