色谱技术在扁桃营养成分与食品农兽药残留分析中的应用
|
摘要
全文包括三部分。
第一部分：绪论
阐述了色谱及其相关前处理技术在食品营养成分及农兽药残留分析中的应用，并对世界著名干果扁桃的国内外研究状况进行了论述。
第二部分：色谱技术在扁桃营养成分分析中的应用
首次用氨基酸自动分析仪对陕西蒲城产13#扁桃仁中的氨基酸含量进行了分析。结果表明，18种氨基酸总量为23.210％，8种人体必需氨基酸种类齐全，总含量为6.857％，其它一些具有药理作用的活性氨基酸如谷氨酸、精氨酸、天冬氨酸、甘氨酸、组氨酸等含量也很丰富。
首次研究了超声波强化提取扁桃油的工艺条件，优化条件为：超声波功率250W、频率40KHz，石油醚提取，种仁粒度40目，浸泡时间36h，超声时间0.5h，溶剂量1：9(W／V)。该条件下，扁桃油提取率高达58.55％。首次用GC-MS法对陕西蒲城产扁桃油的脂肪酸组成进行了分析，并对扁桃油的理化特性进行了表征。结果表明，扁桃油含有5种脂肪酸，其中，饱和脂肪酸——硬脂酸和棕榈酸，总量不足9.0％，不饱和脂肪酸——油酸、亚油酸以及少量的9-十六碳稀酸(棕榈油酸)总量为91.48～91.87％。扁桃油理化性状良好。
首次建立了扁桃仁中α-V_E的HPLC测定方法，测定了陕西蒲城产扁桃仁和扁桃油中α-V_E的含量。结果表明，扁桃仁中α-V_E的含量为201.2～216.7mg／kg。扁桃油中α-V_E含量为355.11～406.38 mg／kg。
建立了扁桃仁中同时测定4种水溶性维生素Vc、V_(B1)、V_(B2)和V_(B6)的HPLC分析方法，测定了陕西蒲城产扁桃仁中Vc、V_(B1)、V_(B2)和V_(B6)的含量。结果表明，扁桃仁V_(B2)含量为4.27～4.53 mg／kg，V_(B1)含量为0.799～0.838 mg／kg，Vc和V_(B6)未检出。
分析了陕西蒲城产扁桃仁中的水分、灰分、可溶性糖、粗蛋白、粗脂肪、矿质元素等成分。结果表明，扁桃仁水分为4.22～4.70％，灰分为2.84～3.11％，
可溶性还原糖含量为2.53~3.54%，可溶性总糖含量为4.98~5.16%，粗蛋白含
里为26.00~30.56%，粗脂肪含量为51.67~56.67%，人体所需的9种矿质元素
含量丰富，依次为K>P>Mg>ea>Na>Fe>zn>Mn>Cu，属于高K、高Ca、
富Fe、富zn食品，不含pb、Cd、Hg、As等有害元素。
第三部分:色谱技术在食品农兽药残留分析中的应用
首次建立了SPE-HPLC法同时测定鸡蛋粉中12种磺胺类药物残留的分析方
法。该法在等度洗脱下22min之内完成了12种磺胺类药物和样品杂质的分离。
检出限在0.002~0.045林g/g，完全满足国际食品法典委员会(CAC)及欧盟、美
国、日本和韩国等国家对食品中磺胺类药物最大残留限量规定的检测要求。当添
加水平在0.1一1 .0林创g时，12种磺胺类药物平均回收率在71 .13士5.02%~
99.53士5.13%之间，达到了出口食品中残留分析方法质量控制规范要求。目前正
在申报国家行业标准。
首次建立了sPME-口c技术同时测定浓缩苹果汁样品中8种有机磷农药残留
的方法，检出限在4.0~4In叭g之间，完全满足且高于国际食品法典委员会
(CAC)及欧盟、美国、日本和韩国等国家对食品中有机磷类农药最大残留限量
规定的检出要求。当添加水平在0.8一10.0协叭g时，8种有机磷平均回收率在
69.24到.18%~103.1肚3.68%之间，完全满足出口食品残留分析质t控制规范方
法要求。目前正在申报国家行业标准。
The thesis includes three parts.
Part I: Review
A review of the application of the chromatography and interrelated sample pretreatment technologies in analysis of nutrient components and residues for pesticides and veterinary drugs in foods and the research status quo in home and abroad about almond-a famous nut food.
Part II: Application of chromatography in analysis of almond's
nutrient components
The amino acids in 13# almond kernel in Shanaxi Pucheng were analyzed by amino acid analyzer for the first time. The results indicated that there are 23.210% eighteen amino acids and 6.857% eight amino acids being indispensable to body in the almond kernel, and other active amino acids such as glutamic acid, arginine, aspartic acid, glycin, histidine are also rich in it.
The optimal condition on extraction almond oil was established for the first time. Under the optical condition as follows: the power of ultrasonic wave 250W, frequency 40KHz, extraction by petroleum ether, material granularity 40mu, immersed time 36h, ultrasonic time 0.5h, solvent ratio 1:9 (W/V), the yield of 58.55% of almond oil was achieved. The fatty acids composition in Shannxi Pucheng almond oil was also analyzed by gas chromatography- mass spectrum (GC-MS) first. The results showed that the five kinds of fatty acids which include two saturated fatty acids (Octadecanoic acid and Hexadecanoic acid) that total content fall short of 9.0% and three unsaturated fatty acids (Oleic acid, 8,11-Octadecadienoic acid, and a small
quantity of 9-Hexadecenoic acid) that take up 91.48-91.87% of the all were discovered in the oil. The physical - chemical characterization of the oil was proved to be fine.
The new method with high performance liquid chromatography (HPLC) for determining a- tocopherol in almond was set up. The results of determination of the almond in Shannxi Pucheng showed that there are 201.2~216.7mg/kg a- tocopherol in the kernel and 355.11 ~406.38 mg/kg a- tocopherol in the oil.
The method with HPLC for determining vitamin C, vitamin Bl, vitamin B2 and vitamin B6 in almond was established. The results of determination of the almond in Shannxi Pucheng indicated that there are 4.27~4.53 mg/kg vitamin B2 and 0.799~ 0.838 mg/kg vitamin B1, and that vitamin C and vitamin B6 were not discovered in the kernel.
The other components including moisture, ash, soluble sugar, crude protein, crude oil and mine elements in Shannxi Pucheng almond kernel were analyzed. The results showed that there are 4.22~4.70% moisture, 2.84~3.11% ash, 2.53~3.54% soluble deoxidized sugar, 4.98~5.16% soluble total sugar, 26.00~30.56% crude protein, 51.67~56.67% crude oil and nine abundant mine elements which content is K > P > Mg > Ca > Na > Fe > Zn > Mn > Cu, especially richer in Fe , Zn , K and Ca than some familiar nuts, and that the harmful elements -Pb, Cd,, Hg, As were not discovered in the kernel. So the almond belongs to a kind of excellent food.
Part III. Application of chromatography in analysis of residues for
pesticides and veterinary drugs in foods
The method with solid-phase extraction(SPE) coupled with HPLC (SPE-HPLC) for the simultaneous determination of the twelve sulfonamides residues in egg powder has been established for the first time. The twelve sulfonamides and impurity in sample were completely separated in 22 min with isocratic elution. The 0.002-0.045mg/kg of limits of detection of the method for twelve sulfonamides were gained, which satisfy the requirements of detection the Maximum Residue Limits (MRL) of sulfonamides prescribed by CAC and Europe Union Organization (EUC)
and some countries such as USA, Japan and Corea in foodstuffs. When added levels ranged between 0.1 g/g and 1.0 g/g standards, the average recoveries of 71.13 5.02%~99.53 5.13% to all sulfonamides in the sample were obtained, which accorded with the detection criterion of quality-control standardization in residues analysis. At present, this method is being declared country industry standard.
The new method with solid-phase microextraction (SPME) coupled with gas chro
第一部分：绪论
阐述了色谱及其相关前处理技术在食品营养成分及农兽药残留分析中的应用，并对世界著名干果扁桃的国内外研究状况进行了论述。
第二部分：色谱技术在扁桃营养成分分析中的应用
首次用氨基酸自动分析仪对陕西蒲城产13#扁桃仁中的氨基酸含量进行了分析。结果表明，18种氨基酸总量为23.210％，8种人体必需氨基酸种类齐全，总含量为6.857％，其它一些具有药理作用的活性氨基酸如谷氨酸、精氨酸、天冬氨酸、甘氨酸、组氨酸等含量也很丰富。
首次研究了超声波强化提取扁桃油的工艺条件，优化条件为：超声波功率250W、频率40KHz，石油醚提取，种仁粒度40目，浸泡时间36h，超声时间0.5h，溶剂量1：9(W／V)。该条件下，扁桃油提取率高达58.55％。首次用GC-MS法对陕西蒲城产扁桃油的脂肪酸组成进行了分析，并对扁桃油的理化特性进行了表征。结果表明，扁桃油含有5种脂肪酸，其中，饱和脂肪酸——硬脂酸和棕榈酸，总量不足9.0％，不饱和脂肪酸——油酸、亚油酸以及少量的9-十六碳稀酸(棕榈油酸)总量为91.48～91.87％。扁桃油理化性状良好。
首次建立了扁桃仁中α-V_E的HPLC测定方法，测定了陕西蒲城产扁桃仁和扁桃油中α-V_E的含量。结果表明，扁桃仁中α-V_E的含量为201.2～216.7mg／kg。扁桃油中α-V_E含量为355.11～406.38 mg／kg。
建立了扁桃仁中同时测定4种水溶性维生素Vc、V_(B1)、V_(B2)和V_(B6)的HPLC分析方法，测定了陕西蒲城产扁桃仁中Vc、V_(B1)、V_(B2)和V_(B6)的含量。结果表明，扁桃仁V_(B2)含量为4.27～4.53 mg／kg，V_(B1)含量为0.799～0.838 mg／kg，Vc和V_(B6)未检出。
分析了陕西蒲城产扁桃仁中的水分、灰分、可溶性糖、粗蛋白、粗脂肪、矿质元素等成分。结果表明，扁桃仁水分为4.22～4.70％，灰分为2.84～3.11％，
可溶性还原糖含量为2.53~3.54%，可溶性总糖含量为4.98~5.16%，粗蛋白含
里为26.00~30.56%，粗脂肪含量为51.67~56.67%，人体所需的9种矿质元素
含量丰富，依次为K>P>Mg>ea>Na>Fe>zn>Mn>Cu，属于高K、高Ca、
富Fe、富zn食品，不含pb、Cd、Hg、As等有害元素。
第三部分:色谱技术在食品农兽药残留分析中的应用
首次建立了SPE-HPLC法同时测定鸡蛋粉中12种磺胺类药物残留的分析方
法。该法在等度洗脱下22min之内完成了12种磺胺类药物和样品杂质的分离。
检出限在0.002~0.045林g/g，完全满足国际食品法典委员会(CAC)及欧盟、美
国、日本和韩国等国家对食品中磺胺类药物最大残留限量规定的检测要求。当添
加水平在0.1一1 .0林创g时，12种磺胺类药物平均回收率在71 .13士5.02%~
99.53士5.13%之间，达到了出口食品中残留分析方法质量控制规范要求。目前正
在申报国家行业标准。
首次建立了sPME-口c技术同时测定浓缩苹果汁样品中8种有机磷农药残留
的方法，检出限在4.0~4In叭g之间，完全满足且高于国际食品法典委员会
(CAC)及欧盟、美国、日本和韩国等国家对食品中有机磷类农药最大残留限量
规定的检出要求。当添加水平在0.8一10.0协叭g时，8种有机磷平均回收率在
69.24到.18%~103.1肚3.68%之间，完全满足出口食品残留分析质t控制规范方
法要求。目前正在申报国家行业标准。
The thesis includes three parts.
Part I: Review
A review of the application of the chromatography and interrelated sample pretreatment technologies in analysis of nutrient components and residues for pesticides and veterinary drugs in foods and the research status quo in home and abroad about almond-a famous nut food.
Part II: Application of chromatography in analysis of almond's
nutrient components
The amino acids in 13# almond kernel in Shanaxi Pucheng were analyzed by amino acid analyzer for the first time. The results indicated that there are 23.210% eighteen amino acids and 6.857% eight amino acids being indispensable to body in the almond kernel, and other active amino acids such as glutamic acid, arginine, aspartic acid, glycin, histidine are also rich in it.
The optimal condition on extraction almond oil was established for the first time. Under the optical condition as follows: the power of ultrasonic wave 250W, frequency 40KHz, extraction by petroleum ether, material granularity 40mu, immersed time 36h, ultrasonic time 0.5h, solvent ratio 1:9 (W/V), the yield of 58.55% of almond oil was achieved. The fatty acids composition in Shannxi Pucheng almond oil was also analyzed by gas chromatography- mass spectrum (GC-MS) first. The results showed that the five kinds of fatty acids which include two saturated fatty acids (Octadecanoic acid and Hexadecanoic acid) that total content fall short of 9.0% and three unsaturated fatty acids (Oleic acid, 8,11-Octadecadienoic acid, and a small
quantity of 9-Hexadecenoic acid) that take up 91.48-91.87% of the all were discovered in the oil. The physical - chemical characterization of the oil was proved to be fine.
The new method with high performance liquid chromatography (HPLC) for determining a- tocopherol in almond was set up. The results of determination of the almond in Shannxi Pucheng showed that there are 201.2~216.7mg/kg a- tocopherol in the kernel and 355.11 ~406.38 mg/kg a- tocopherol in the oil.
The method with HPLC for determining vitamin C, vitamin Bl, vitamin B2 and vitamin B6 in almond was established. The results of determination of the almond in Shannxi Pucheng indicated that there are 4.27~4.53 mg/kg vitamin B2 and 0.799~ 0.838 mg/kg vitamin B1, and that vitamin C and vitamin B6 were not discovered in the kernel.
The other components including moisture, ash, soluble sugar, crude protein, crude oil and mine elements in Shannxi Pucheng almond kernel were analyzed. The results showed that there are 4.22~4.70% moisture, 2.84~3.11% ash, 2.53~3.54% soluble deoxidized sugar, 4.98~5.16% soluble total sugar, 26.00~30.56% crude protein, 51.67~56.67% crude oil and nine abundant mine elements which content is K > P > Mg > Ca > Na > Fe > Zn > Mn > Cu, especially richer in Fe , Zn , K and Ca than some familiar nuts, and that the harmful elements -Pb, Cd,, Hg, As were not discovered in the kernel. So the almond belongs to a kind of excellent food.
Part III. Application of chromatography in analysis of residues for
pesticides and veterinary drugs in foods
The method with solid-phase extraction(SPE) coupled with HPLC (SPE-HPLC) for the simultaneous determination of the twelve sulfonamides residues in egg powder has been established for the first time. The twelve sulfonamides and impurity in sample were completely separated in 22 min with isocratic elution. The 0.002-0.045mg/kg of limits of detection of the method for twelve sulfonamides were gained, which satisfy the requirements of detection the Maximum Residue Limits (MRL) of sulfonamides prescribed by CAC and Europe Union Organization (EUC)
and some countries such as USA, Japan and Corea in foodstuffs. When added levels ranged between 0.1 g/g and 1.0 g/g standards, the average recoveries of 71.13 5.02%~99.53 5.13% to all sulfonamides in the sample were obtained, which accorded with the detection criterion of quality-control standardization in residues analysis. At present, this method is being declared country industry standard.
The new method with solid-phase microextraction (SPME) coupled with gas chro
引文
1．郑建山编著．功能性食品[J]．第一卷．中国轻工业出版社．2001，1～5．
2．沈同，王镜岩．生物化学[M]．高等教育出版社．第二版，1990：74～109．
3．大连轻工业学院，华南理工大学，郑州轻工业学院等合编．食品科学[M]．中国轻工业出版社．1994：240～242．
4．刘惠文．氨基酸和生物资源[J]．1995，17(2)：50～55．
5．李芳，史霄燕．色谱[J]．1995，13(3)：200～202．
6. L. Campanella, G.Crescentini, P. Avino. Journal of Chromatography A, 833 (1999):137～145.
7. David M. Albin, Jennifer E. Wubben, Vince M.Gabert. Animal Feed Science and Technology.87 (2000) 173±186.
8．蒋新宇．周春山．湖南化工[J]．1999，29(2)：9～11．
9. Mare Roth.ANALYTICAL CHEMISTRY[J], 1971,43 (7) : 880～882.
10. Kang-Lyung Woo,Young-Kyoo Ahan. Journal of Chromatography A,740 (1996) 41～45.
11. L.Campanella, G.Ctescentini, P.Avino, J.Chromatogr., 1999,833, 137.
12．周建华．山东轻工业学院学报[J]．1998，12(4)：48～50．
13．许庆秦．山西师范大学学报[J]．2002，16(1)：49～51．
14．孟庆国，张铁恒．数理统计与管理[J]．1998，17(3)：4～6．
15．孟庆国，王培承，李珍萍等．分析化学[J]．1998，26(5)：517～519．
16．孟庆国，赵风兰，张炳真．分析化学[J]．2000，28(1)：130～132．
17. Akira Namere, Mikio Yashiki, Manami Nishida, et al. Journal of Chromatography B, 776(2002) 49～55.
18．刘江虹，刘国请，尹家元等．云南化工[J]．2001，28(2)：17～21．
19．孙远明，余群力主编．食品营养学[M]．中国农业大学出版社．北京．2002： 85～108．
20. P. Moreno, V. Salvado. Journal of Chromatography A, 870 (2000) 207～215.
21．陈红，吴樱．生物学杂志[J]．2002，19(3)：37～38．
22．金米聪，王立，符展明．色谱[J]．2001，19(5)：478～480．
23．高燕红，许秀敏．中国卫生检验杂志[J]．2002，12(5)：553．
24．汤丽芬，陈红英，林敬本等．华南预防医学[J]．2002，28(3)：40～41．
25．杨亚玲，孟冬玲，孙海林等．云南化工[J]．2003，30(2)：28～30．
26．沈小碗主编．色谱法在食品分析中的应用[M]．北京大学出版社．1991．
27．胡晓形．农药[J]．1998，37(6)：7～10．
28．陈君石．预防医学文献信息[J]．2003，9(2)：254～256．
29．胡晓宁，苏诚玉．甘肃科技纵横[J]．2003，32(3)：15～16．
30. Lopez T L, Garcia M D G, Vidal J L M, et al. Anal.Chim.Acta, 2001,447 : 101～111.
31. EDGELL K W. J.Assoc off Anal Chem. 1991, 74:309～312.
32．高如瑜，赵静辉．农药[J]．1997，36(9)：28．
33．张洪兰．色谱[J]．1997，15(5)：442～444．
34. Wal J M. J Assoc of Anal Chem.1980,63 (5) : 1044～1048.
35．将定国，杨大进，方从容等．中国食品卫生杂志[J]．2003，15(1)：36～38．
36．农业部畜牧兽医局．中国兽药杂志[J]．2002，36(7)：13～14．
37. G. Stoev, Al Michailova. Journal of Chromatography A, 871 (2000) 37～42.
38. M.C.Hennion, Trends Anal.Chem., 1991, 10:317.
39．张莘民，杨凯．中国环境监测[J]．2000，16(6)：54～57
40. E.M. Thurman, Kirk Snavely .Trends in Analytical Chemistry, 2000,19 (1):18～26.
41. Guidotti Maurizio, Ravaioli Guido, et al. J.Chromatography.1999,22(7): 414～416.
42．刘振玲，吴采樱．药学学报[J]．2003，38(2)：153～158．
43. Takeshi Kumazawa, Hirosh Seno, Xiao-pen Lee et al. Analytica chimica Acta. 1999,387:53.
44. Lee XP, Kumazawa Takeshi, Sato Keizo. J chromatogr Sci,1997, 35:302.
45. Stypinski D,Wiebe LI Mercer TR.. J Pharm Biomed Anal, 1998, 16 (6): 1067～1073.
46. Barr DB, Ashlry DL.J Anal Toxicol. 1998,22 (2): 96～104.
47. Kulezykowsksa E, Ivone PM.J Chromatogr Sci. 1998,35 (4) : 175～178.
48．王新春，阳长明，侯世祥等．中国医院药学杂志[J]．2001，21(12)：747～748．
49. Pag B D, Lacroix G. J Chromatogr. 2000,873 : 79.
50. Vercauteren J Demeester A.Desmaele T et al. J.Anal.Atom.Sprctr 2000, 873 : 117.
51. D Andrzejewski, A Weisz, J.Chromatogr A, 1999,863:37.
52．姜会书，徐会君．农业与技术[J]，1999，19(6)：35～37．
53. Colin F. Poole, Ajith D.Gunatilleka, Revathy Sethuraman.J.Chromatogz.A, 885 (2000):17～39.
54．张海霞，朱彭龄．分析化学[J]，2000，28(9)：1172～1180．
55．姜会书，徐会君．农业与技术[J]．1999，19(6)：35～37．
56. Pena F, Cardenas S, Gallego M, Valcarcel M J.Talanta, 2002,56:727～734.
57. Rodriguez R, Pieo Y, Font G, Manes J. J.Chromatogr.A, 2001, 924:387～396
58. Delgado SMJ, Barroso RS, Femandez-Tostado G. J.Chromtagr.A, 2001, 921 : 287～296
59. Jimenez JJ, Bernal JL, Nozal MJ, ToribioL, AriasE. J.Chromatogr.A, 2001, 919:147～156
60. Soleas GJ, Yan J, Hom K, Goldberg DM. J.Chromatogr.A, 2000, 882 : 205～212
61．刘长武，刘潇威，刘风枝等．色谱[J]．2003，21(3)：255～257．
62．陈毓芳．分析测试学报[J]．2003，22(3)：97～99．
63．林海丹，谢守新，冯德雄等．分析测试学报[J]．2003，22(1)：94～96．
64. W. Hela, M. Brandtner, R. Widek, R. Schuh. Food Chemistry 83 (2003) : 601～608.
65．康莉，仲岳桐，陈春晓等．中国卫生检验杂志[J]．2003，12(1)：53～54．
66．谢孟峡，刘嫒，蒋敏．分析化学[J]．2002，30(11)：1308～1311．
67．葛宝坤，王云凤，常春艳等．分析测试学报[J]．2003，22(5)：91～93
68. Ming-Ren S. Fuh, Shun-An Chan. Talanta 55 (2001) :1127～1139.
69. ARTHURCL, PAWLISZYNJ. J.Anal.Chem., 1990, 62: 2145.
70. Arthurel, Killarnlm, Buehdzkd, et al.J.AnalChem, 1992, 64: 1960～342.
71. ZHANGZ, YANGMJ, PAWLISZYNJ. J.Anal.Chem., 1994, 66 (17): 844A～853A.
72. J Pawliszyn. J Chromatogr, Sci., 2000,38 : 270.
73. Chenj, Pawliszynj. J.Anal.Chem, 1995,67 (15) : 2530～2533.
74. SenNP, StephenWS, PageBD. J.Chromatogr.A, 1997, 788 : 131～140.
75．贾金平，何翊，黄骏雄．化学进展[J]．1998，10(1)：74～84．
76．栾天罡，张展霞．分析化学[J]．2003，31(4)：496～500．
77. R.Eisert, K.Levsen, Fresenius .J.Anal.Chem..351 (1995) : 555～560.
78. Eisert R. et al. J.Am.Soc.Mass spectrum., Nov 1995, 6 (11) : 1119～1130.
79. I.Valor, J.C.Molto, D.Apraiz etc. J.Chromatogr.A, 767 (1997) : 195～203.
80．王新平．化学研究与应用[J]．2003，15(2)：136～137．
81. Y.C.Ling, I.P.Huang. J.Chromatographia .40 (1995) : 259.
82. Bruce A. Tomkins, Angela R. Barnard. J.Chromatogr.A, 964 (2002) : 21～33,
83. Sonia Magdic, Janusz B.Pawliszyn. J.Chromatogr.A, 723 (1996) : 111～122
84. J.P. Perez-Trujillo, S. Frias, J.E. Conde, et al. J.Chromatogr.A, 963 (2002): 95～105.
85. C. Aguilar, A. Penalver, E. Pocurull et al. J.Chromatogn.A, 844 (1999) : 425～432.
86. M.Vitali, M.Guidotti, P.Giovinazzo et al. Food Addit.Contam.280 (1998): 280.
87. EvansTJ, ButzkeCE, EbelerSE.J.Chromatogr.A, 1997, 786:293～298.
88. Castro J, Perez R A, Sanehez-BruneteC, TadeoJL.J.Chromatographia, 2001,53 (2):361～365.
89. Ana Luisa Simplicio, Luis Vilas Boas. J.Chromatogr.A, 833 (1999) : 35～42.
90. M.Fernandez, C.Padron, L.Marconi et al. J.Chromatogr.A, 922 (2001) : 257～265.
91. Natalia Fidalgo-Used, Giuscppe Centineo et al. J.Chromatogr.A, 1017 (2003) : 35～44.
92．郭春会，梅立新，张檀等．扁桃的园艺技术[M]．中国标准出版社．2001：1～8．
93．朱京琳．新疆巴旦杏[M]．乌鲁木齐：新疆人民出版社，1984．
94．玛依拉，李阿峰．中国民族民间医药杂志[J]．2001，12：163～164．
95．刘勇民．维吾尔药志[J]．新疆人民出版社．1984．
96．顾永寿等译．维吾尔医用常用药材[J]．新疆科技卫生出版社．1992．
97．张云涛．世界农业[J]．1999，7：31～32．
98. Cruess, W. V., Kiibuck, J. H., & Hahl, E.. Fruit Products Journal, 1947, 26 : 363～365.
99. Gordon, M. H. Natural Product Reports, 1996:265～273.
100. Ames, B. M.. Science, 1983, 221:1256～1264.
101. Steinberg, D. Atherosclerosis Review, 1992, 18:1～6.
102. Rikher, A.A,; Kriventsov, V.I.Fiziol Rast.1980, 27 (4): 729～734.
103. Youle,Richard L.;Huang,Anthony H,C. Am.J.Bot.1981,68 (1): 44～48.
104．成健红，侯平，李疆等．干旱区研究[J]．2000,17(1)：32～38．
105. Saura Calixto F.; Canellas J. J, Sci.Food Agric.1982,33 (4): 336～339.
106. Saura Calixto, F.; Canellas, J. I.Lebensm.-Unter.Forsch.1982,175 (1): 34～37.
107. Saura Calixto, F.; Canellas, J., Garcia-Raso, A., J.Agric.Food Chem. 1984,32: 1018～1021.
108. Soler, L., Canellas,J., Saura-Calixto,F.,. J.Agric.Food Chem. 1989,37:1400～1404.
109. Rikher, A.A,; Pyzhov, V.Kh. Applied Biochemistry and Microbiology. 1987, 23: 96～105.
110. Sathe, S.K. Journal of Food Biocheraistry. 1993,16: 249～264.
111. K.W.C.Sze-Tao, S.K.Sathe.Food Chemistry 2000,69 : 153～160.
112. Sathe SK, Wolf W J, Roux KH.et al. J.Agric.Food Chem. 2002, 50 (15): 4333～4341.
113. Davis, PA Iwahashi, CK. Cancer letters. 2001, 165 (1) :27～33.
114．朱京琳．新疆巴旦杏[M]．乌鲁木齐市疆人民出版社：1984，4．
115. Hyson DA, Schneeman BO, Davis PA. The Journal of Nutrition. 2002,132 (4): 703-707.
116. E.MICKLANDERL, BRIMERS.B. ENGELSEN. Applied Spectroscopy. 2002, 56 (9):1139～1146.
117. Mandenius, C F; Bueloe,L; Danielsson, B. Acta. Chem. Scand, Ser. B. 1983, B 37 (8):739～742.
118. Arya, S.S.; Madhura,C.V.J. Food Sci. Technol, 1986,23 (2): 100～101.
119. Lacourse, William R.; Krull, Iras. Anal. Chem. 1987,59 (1): 49～53.
120. Femenia A, Garcia-Marin M, Simal S. et al. J. Agric. Food Chem. 2001, 49 (12): 5828～5834.
121. Samah Allam, SM. Assiut Journal of Agricultural Sciences. 2001, 32 (1). 37～47.
122. Sanehez-Vizcaino,E.; Rios,R.Moreno. World Congr. Anim. Feed. 1978,7 (1): 487～91.
123. Frison-Norrie S, Sporns P. J. Agric. Food Chem. 2002, 50 (10): 2782～2787.
124. Sang SM, Lapsley K, Jeong WS.et al. J. Agric. Food Chem. 2002, 50 (8): 2459～2463.
125. Sang SM, Lapsley K, Rosen RT. et al. J. Agric. Food Chem., 2002, 50 (3): 607～609.
126. Sang SM, Cheng XF, Hui-Yin Fu .et al, Tetrahedron Letters. 2002, 43 (14): 2547～2549.
127. Sang SM, Kikuzaki H, Lapsley K. J. Agric. Food Chem. 2002, 50 (16): 4709～4712.
128. M. Pinelo, M. Rubilar, J. Sineiro et al. Food Chemistry.85 (2004): 267～273.
129. Wood, J. E., Senthilmohan, S. T., & Peskin, A. V. Food Chemistry, 2002, 77: 155～161.
130. Christopher A. Toles, Wayne E. Marshall, Lynda H. Wartelle.et al. Bioresource Technology 75 (2000) :197±203.
131．李新明．新疆林业[J]．2003，4：26～27．
132．韩宏伟，王建友等．经济林研究[J]．2003，21(1)：42～44．
133．徐胜利，陈小青．山西果树[J]．2003(3)：52～52．
134．牛云，赵明等．北方果树[J]．2002，6：22～24
135．张天锡．新疆林业[J]．2002，5：28～29．
136．孙志红，李保国等．巴州科技[J]．2002，2：11～14．
137．成健红，谭敦炎等．西北植物学报[J]．2001，21(5)：894～899，T001．
138．杨绍彬，刘福权．经济林研究[J]．2000，18(3)：41～42．
139．李利民，卢春生．中国农学通报[J]．1999,15(1)：20～22，29．
140．成健红，马木提．干旱区研究[J]．2000，17(1)：32～38．
141．张凤云，王国礼，张和平等．西北农业学报[J]．1997，6(3)：82～84．
142．张凤云，毛富春，翟梅枝．中国林福特产[J]．2000，3：1～2．
143．张凤云，毛富春，杨秀平．西北农业学报[J]．2000，9(3)：83～85．
144．刘金荣，但建明，江发寿等．营养学报[J]．2002，2 4(2)：202～203．
145．刘金荣，但建明，赵文彬等．微量元素与健康研究[J]．2002，19(1)：29～30．
146．解成喜，王强，谢效新．新疆大学学报(自然科学版)[J]．2003，20(1)：99～100．
147．钱秀英，张玉萍．新疆大学学报(自然科学版)[J]．2002，19(4)：437～440．
148．高疆生，易晓华，陈毓荃等．西北农业学报[J]．2001，10(1)：11～13．
149．高疆生，易晓华，陈毓荃等．西北农业学报[J]．2001，10(2)：36～38．
150．永本典生等．国外医药中医中药分册[J]．1989，11(6)：23～24．
151．邓淑文，肖碧玉，马龙等．营养学报[J]．1998，20(2)：234～235．
152．肖碧玉，邓淑文，马龙等．中国老年学杂志[J]．1996，16(5)：291～292．
153．肖颖，王军波，闫少芳等．中国公共卫生[J]．2002，18(8)：931～932．
154．马龙，邓淑文，肖碧玉等．新疆医学院学报[J]．1997，20(2)：92～94．
155. Ma Rc, Oliveira M.. Mol genet-genomies[J]. 2002, 267 (1): 8～71.
156. Rong-Cai Ma M.. Sexplant Reprod[J]. 2001, 14: 163 167.
157. Grane Teruel N, Luna Amador MC, Prats Moya MS.et al. Food Chemistry[J]. 1999, 65 (1):23～28.
158. Seron LH, Poveda EG, Moya MS.et al. Food Chemistry[J]. 1998, 61 (4): 455～459.
159. Abdailah A, Ahurnada MH,Gradziel TM. Journal of the American Society for HorticulturalScience.1998, 123 (6): 1029～1033,
160. Prats Moya S, Grane Teruel N, Berenguer Navarro V.et al. J.Agric.Food Chem. 1997, 45 (6):2093～2097.
161. George D. Nanos, Ioarmis Kazantzis, Panagiotis Kefalas.et al. Scientia Horticulturae[J] .96(2002): 249～256.
2．沈同，王镜岩．生物化学[M]．高等教育出版社．第二版，1990：74～109．
3．大连轻工业学院，华南理工大学，郑州轻工业学院等合编．食品科学[M]．中国轻工业出版社．1994：240～242．
4．刘惠文．氨基酸和生物资源[J]．1995，17(2)：50～55．
5．李芳，史霄燕．色谱[J]．1995，13(3)：200～202．
6. L. Campanella, G.Crescentini, P. Avino. Journal of Chromatography A, 833 (1999):137～145.
7. David M. Albin, Jennifer E. Wubben, Vince M.Gabert. Animal Feed Science and Technology.87 (2000) 173±186.
8．蒋新宇．周春山．湖南化工[J]．1999，29(2)：9～11．
9. Mare Roth.ANALYTICAL CHEMISTRY[J], 1971,43 (7) : 880～882.
10. Kang-Lyung Woo,Young-Kyoo Ahan. Journal of Chromatography A,740 (1996) 41～45.
11. L.Campanella, G.Ctescentini, P.Avino, J.Chromatogr., 1999,833, 137.
12．周建华．山东轻工业学院学报[J]．1998，12(4)：48～50．
13．许庆秦．山西师范大学学报[J]．2002，16(1)：49～51．
14．孟庆国，张铁恒．数理统计与管理[J]．1998，17(3)：4～6．
15．孟庆国，王培承，李珍萍等．分析化学[J]．1998，26(5)：517～519．
16．孟庆国，赵风兰，张炳真．分析化学[J]．2000，28(1)：130～132．
17. Akira Namere, Mikio Yashiki, Manami Nishida, et al. Journal of Chromatography B, 776(2002) 49～55.
18．刘江虹，刘国请，尹家元等．云南化工[J]．2001，28(2)：17～21．
19．孙远明，余群力主编．食品营养学[M]．中国农业大学出版社．北京．2002： 85～108．
20. P. Moreno, V. Salvado. Journal of Chromatography A, 870 (2000) 207～215.
21．陈红，吴樱．生物学杂志[J]．2002，19(3)：37～38．
22．金米聪，王立，符展明．色谱[J]．2001，19(5)：478～480．
23．高燕红，许秀敏．中国卫生检验杂志[J]．2002，12(5)：553．
24．汤丽芬，陈红英，林敬本等．华南预防医学[J]．2002，28(3)：40～41．
25．杨亚玲，孟冬玲，孙海林等．云南化工[J]．2003，30(2)：28～30．
26．沈小碗主编．色谱法在食品分析中的应用[M]．北京大学出版社．1991．
27．胡晓形．农药[J]．1998，37(6)：7～10．
28．陈君石．预防医学文献信息[J]．2003，9(2)：254～256．
29．胡晓宁，苏诚玉．甘肃科技纵横[J]．2003，32(3)：15～16．
30. Lopez T L, Garcia M D G, Vidal J L M, et al. Anal.Chim.Acta, 2001,447 : 101～111.
31. EDGELL K W. J.Assoc off Anal Chem. 1991, 74:309～312.
32．高如瑜，赵静辉．农药[J]．1997，36(9)：28．
33．张洪兰．色谱[J]．1997，15(5)：442～444．
34. Wal J M. J Assoc of Anal Chem.1980,63 (5) : 1044～1048.
35．将定国，杨大进，方从容等．中国食品卫生杂志[J]．2003，15(1)：36～38．
36．农业部畜牧兽医局．中国兽药杂志[J]．2002，36(7)：13～14．
37. G. Stoev, Al Michailova. Journal of Chromatography A, 871 (2000) 37～42.
38. M.C.Hennion, Trends Anal.Chem., 1991, 10:317.
39．张莘民，杨凯．中国环境监测[J]．2000，16(6)：54～57
40. E.M. Thurman, Kirk Snavely .Trends in Analytical Chemistry, 2000,19 (1):18～26.
41. Guidotti Maurizio, Ravaioli Guido, et al. J.Chromatography.1999,22(7): 414～416.
42．刘振玲，吴采樱．药学学报[J]．2003，38(2)：153～158．
43. Takeshi Kumazawa, Hirosh Seno, Xiao-pen Lee et al. Analytica chimica Acta. 1999,387:53.
44. Lee XP, Kumazawa Takeshi, Sato Keizo. J chromatogr Sci,1997, 35:302.
45. Stypinski D,Wiebe LI Mercer TR.. J Pharm Biomed Anal, 1998, 16 (6): 1067～1073.
46. Barr DB, Ashlry DL.J Anal Toxicol. 1998,22 (2): 96～104.
47. Kulezykowsksa E, Ivone PM.J Chromatogr Sci. 1998,35 (4) : 175～178.
48．王新春，阳长明，侯世祥等．中国医院药学杂志[J]．2001，21(12)：747～748．
49. Pag B D, Lacroix G. J Chromatogr. 2000,873 : 79.
50. Vercauteren J Demeester A.Desmaele T et al. J.Anal.Atom.Sprctr 2000, 873 : 117.
51. D Andrzejewski, A Weisz, J.Chromatogr A, 1999,863:37.
52．姜会书，徐会君．农业与技术[J]，1999，19(6)：35～37．
53. Colin F. Poole, Ajith D.Gunatilleka, Revathy Sethuraman.J.Chromatogz.A, 885 (2000):17～39.
54．张海霞，朱彭龄．分析化学[J]，2000，28(9)：1172～1180．
55．姜会书，徐会君．农业与技术[J]．1999，19(6)：35～37．
56. Pena F, Cardenas S, Gallego M, Valcarcel M J.Talanta, 2002,56:727～734.
57. Rodriguez R, Pieo Y, Font G, Manes J. J.Chromatogr.A, 2001, 924:387～396
58. Delgado SMJ, Barroso RS, Femandez-Tostado G. J.Chromtagr.A, 2001, 921 : 287～296
59. Jimenez JJ, Bernal JL, Nozal MJ, ToribioL, AriasE. J.Chromatogr.A, 2001, 919:147～156
60. Soleas GJ, Yan J, Hom K, Goldberg DM. J.Chromatogr.A, 2000, 882 : 205～212
61．刘长武，刘潇威，刘风枝等．色谱[J]．2003，21(3)：255～257．
62．陈毓芳．分析测试学报[J]．2003，22(3)：97～99．
63．林海丹，谢守新，冯德雄等．分析测试学报[J]．2003，22(1)：94～96．
64. W. Hela, M. Brandtner, R. Widek, R. Schuh. Food Chemistry 83 (2003) : 601～608.
65．康莉，仲岳桐，陈春晓等．中国卫生检验杂志[J]．2003，12(1)：53～54．
66．谢孟峡，刘嫒，蒋敏．分析化学[J]．2002，30(11)：1308～1311．
67．葛宝坤，王云凤，常春艳等．分析测试学报[J]．2003，22(5)：91～93
68. Ming-Ren S. Fuh, Shun-An Chan. Talanta 55 (2001) :1127～1139.
69. ARTHURCL, PAWLISZYNJ. J.Anal.Chem., 1990, 62: 2145.
70. Arthurel, Killarnlm, Buehdzkd, et al.J.AnalChem, 1992, 64: 1960～342.
71. ZHANGZ, YANGMJ, PAWLISZYNJ. J.Anal.Chem., 1994, 66 (17): 844A～853A.
72. J Pawliszyn. J Chromatogr, Sci., 2000,38 : 270.
73. Chenj, Pawliszynj. J.Anal.Chem, 1995,67 (15) : 2530～2533.
74. SenNP, StephenWS, PageBD. J.Chromatogr.A, 1997, 788 : 131～140.
75．贾金平，何翊，黄骏雄．化学进展[J]．1998，10(1)：74～84．
76．栾天罡，张展霞．分析化学[J]．2003，31(4)：496～500．
77. R.Eisert, K.Levsen, Fresenius .J.Anal.Chem..351 (1995) : 555～560.
78. Eisert R. et al. J.Am.Soc.Mass spectrum., Nov 1995, 6 (11) : 1119～1130.
79. I.Valor, J.C.Molto, D.Apraiz etc. J.Chromatogr.A, 767 (1997) : 195～203.
80．王新平．化学研究与应用[J]．2003，15(2)：136～137．
81. Y.C.Ling, I.P.Huang. J.Chromatographia .40 (1995) : 259.
82. Bruce A. Tomkins, Angela R. Barnard. J.Chromatogr.A, 964 (2002) : 21～33,
83. Sonia Magdic, Janusz B.Pawliszyn. J.Chromatogr.A, 723 (1996) : 111～122
84. J.P. Perez-Trujillo, S. Frias, J.E. Conde, et al. J.Chromatogr.A, 963 (2002): 95～105.
85. C. Aguilar, A. Penalver, E. Pocurull et al. J.Chromatogn.A, 844 (1999) : 425～432.
86. M.Vitali, M.Guidotti, P.Giovinazzo et al. Food Addit.Contam.280 (1998): 280.
87. EvansTJ, ButzkeCE, EbelerSE.J.Chromatogr.A, 1997, 786:293～298.
88. Castro J, Perez R A, Sanehez-BruneteC, TadeoJL.J.Chromatographia, 2001,53 (2):361～365.
89. Ana Luisa Simplicio, Luis Vilas Boas. J.Chromatogr.A, 833 (1999) : 35～42.
90. M.Fernandez, C.Padron, L.Marconi et al. J.Chromatogr.A, 922 (2001) : 257～265.
91. Natalia Fidalgo-Used, Giuscppe Centineo et al. J.Chromatogr.A, 1017 (2003) : 35～44.
92．郭春会，梅立新，张檀等．扁桃的园艺技术[M]．中国标准出版社．2001：1～8．
93．朱京琳．新疆巴旦杏[M]．乌鲁木齐：新疆人民出版社，1984．
94．玛依拉，李阿峰．中国民族民间医药杂志[J]．2001，12：163～164．
95．刘勇民．维吾尔药志[J]．新疆人民出版社．1984．
96．顾永寿等译．维吾尔医用常用药材[J]．新疆科技卫生出版社．1992．
97．张云涛．世界农业[J]．1999，7：31～32．
98. Cruess, W. V., Kiibuck, J. H., & Hahl, E.. Fruit Products Journal, 1947, 26 : 363～365.
99. Gordon, M. H. Natural Product Reports, 1996:265～273.
100. Ames, B. M.. Science, 1983, 221:1256～1264.
101. Steinberg, D. Atherosclerosis Review, 1992, 18:1～6.
102. Rikher, A.A,; Kriventsov, V.I.Fiziol Rast.1980, 27 (4): 729～734.
103. Youle,Richard L.;Huang,Anthony H,C. Am.J.Bot.1981,68 (1): 44～48.
104．成健红，侯平，李疆等．干旱区研究[J]．2000,17(1)：32～38．
105. Saura Calixto F.; Canellas J. J, Sci.Food Agric.1982,33 (4): 336～339.
106. Saura Calixto, F.; Canellas, J. I.Lebensm.-Unter.Forsch.1982,175 (1): 34～37.
107. Saura Calixto, F.; Canellas, J., Garcia-Raso, A., J.Agric.Food Chem. 1984,32: 1018～1021.
108. Soler, L., Canellas,J., Saura-Calixto,F.,. J.Agric.Food Chem. 1989,37:1400～1404.
109. Rikher, A.A,; Pyzhov, V.Kh. Applied Biochemistry and Microbiology. 1987, 23: 96～105.
110. Sathe, S.K. Journal of Food Biocheraistry. 1993,16: 249～264.
111. K.W.C.Sze-Tao, S.K.Sathe.Food Chemistry 2000,69 : 153～160.
112. Sathe SK, Wolf W J, Roux KH.et al. J.Agric.Food Chem. 2002, 50 (15): 4333～4341.
113. Davis, PA Iwahashi, CK. Cancer letters. 2001, 165 (1) :27～33.
114．朱京琳．新疆巴旦杏[M]．乌鲁木齐市疆人民出版社：1984，4．
115. Hyson DA, Schneeman BO, Davis PA. The Journal of Nutrition. 2002,132 (4): 703-707.
116. E.MICKLANDERL, BRIMERS.B. ENGELSEN. Applied Spectroscopy. 2002, 56 (9):1139～1146.
117. Mandenius, C F; Bueloe,L; Danielsson, B. Acta. Chem. Scand, Ser. B. 1983, B 37 (8):739～742.
118. Arya, S.S.; Madhura,C.V.J. Food Sci. Technol, 1986,23 (2): 100～101.
119. Lacourse, William R.; Krull, Iras. Anal. Chem. 1987,59 (1): 49～53.
120. Femenia A, Garcia-Marin M, Simal S. et al. J. Agric. Food Chem. 2001, 49 (12): 5828～5834.
121. Samah Allam, SM. Assiut Journal of Agricultural Sciences. 2001, 32 (1). 37～47.
122. Sanehez-Vizcaino,E.; Rios,R.Moreno. World Congr. Anim. Feed. 1978,7 (1): 487～91.
123. Frison-Norrie S, Sporns P. J. Agric. Food Chem. 2002, 50 (10): 2782～2787.
124. Sang SM, Lapsley K, Jeong WS.et al. J. Agric. Food Chem. 2002, 50 (8): 2459～2463.
125. Sang SM, Lapsley K, Rosen RT. et al. J. Agric. Food Chem., 2002, 50 (3): 607～609.
126. Sang SM, Cheng XF, Hui-Yin Fu .et al, Tetrahedron Letters. 2002, 43 (14): 2547～2549.
127. Sang SM, Kikuzaki H, Lapsley K. J. Agric. Food Chem. 2002, 50 (16): 4709～4712.
128. M. Pinelo, M. Rubilar, J. Sineiro et al. Food Chemistry.85 (2004): 267～273.
129. Wood, J. E., Senthilmohan, S. T., & Peskin, A. V. Food Chemistry, 2002, 77: 155～161.
130. Christopher A. Toles, Wayne E. Marshall, Lynda H. Wartelle.et al. Bioresource Technology 75 (2000) :197±203.
131．李新明．新疆林业[J]．2003，4：26～27．
132．韩宏伟，王建友等．经济林研究[J]．2003，21(1)：42～44．
133．徐胜利，陈小青．山西果树[J]．2003(3)：52～52．
134．牛云，赵明等．北方果树[J]．2002，6：22～24
135．张天锡．新疆林业[J]．2002，5：28～29．
136．孙志红，李保国等．巴州科技[J]．2002，2：11～14．
137．成健红，谭敦炎等．西北植物学报[J]．2001，21(5)：894～899，T001．
138．杨绍彬，刘福权．经济林研究[J]．2000，18(3)：41～42．
139．李利民，卢春生．中国农学通报[J]．1999,15(1)：20～22，29．
140．成健红，马木提．干旱区研究[J]．2000，17(1)：32～38．
141．张凤云，王国礼，张和平等．西北农业学报[J]．1997，6(3)：82～84．
142．张凤云，毛富春，翟梅枝．中国林福特产[J]．2000，3：1～2．
143．张凤云，毛富春，杨秀平．西北农业学报[J]．2000，9(3)：83～85．
144．刘金荣，但建明，江发寿等．营养学报[J]．2002，2 4(2)：202～203．
145．刘金荣，但建明，赵文彬等．微量元素与健康研究[J]．2002，19(1)：29～30．
146．解成喜，王强，谢效新．新疆大学学报(自然科学版)[J]．2003，20(1)：99～100．
147．钱秀英，张玉萍．新疆大学学报(自然科学版)[J]．2002，19(4)：437～440．
148．高疆生，易晓华，陈毓荃等．西北农业学报[J]．2001，10(1)：11～13．
149．高疆生，易晓华，陈毓荃等．西北农业学报[J]．2001，10(2)：36～38．
150．永本典生等．国外医药中医中药分册[J]．1989，11(6)：23～24．
151．邓淑文，肖碧玉，马龙等．营养学报[J]．1998，20(2)：234～235．
152．肖碧玉，邓淑文，马龙等．中国老年学杂志[J]．1996，16(5)：291～292．
153．肖颖，王军波，闫少芳等．中国公共卫生[J]．2002，18(8)：931～932．
154．马龙，邓淑文，肖碧玉等．新疆医学院学报[J]．1997，20(2)：92～94．
155. Ma Rc, Oliveira M.. Mol genet-genomies[J]. 2002, 267 (1): 8～71.
156. Rong-Cai Ma M.. Sexplant Reprod[J]. 2001, 14: 163 167.
157. Grane Teruel N, Luna Amador MC, Prats Moya MS.et al. Food Chemistry[J]. 1999, 65 (1):23～28.
158. Seron LH, Poveda EG, Moya MS.et al. Food Chemistry[J]. 1998, 61 (4): 455～459.
159. Abdailah A, Ahurnada MH,Gradziel TM. Journal of the American Society for HorticulturalScience.1998, 123 (6): 1029～1033,
160. Prats Moya S, Grane Teruel N, Berenguer Navarro V.et al. J.Agric.Food Chem. 1997, 45 (6):2093～2097.
161. George D. Nanos, Ioarmis Kazantzis, Panagiotis Kefalas.et al. Scientia Horticulturae[J] .96(2002): 249～256.