【作者】 张萍；

【导师】 申烨华；

【作者基本信息】 西北大学 ， 分析化学， 2004， 硕士

【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2.53³.54%，可溶性总糖含量为4.98⁵.16%，粗蛋白含里为26.00³0.56%，粗脂肪含量为51.67⁵6.67%，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0.002⁰.045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4.0⁴In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。更多还原

【Abstract】 The thesis includes three parts.Part I: ReviewA 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’snutrient componentsThe 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 smallquantity 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 forpesticides and veterinary drugs in foodsThe 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更多还原