【作者】 崔晓明；

【导师】 解成喜；

【作者基本信息】 新疆大学 ， 应用化学， 2004， 硕士

【摘要】 近年来食品中的兽药残留在国内外已成为一个影响广泛和颇具争议的问题，它与公众的健康息息相关，也直接关系到产业界的经济利益。食品中兽药的残留水平一般为1μg~1mg或更低，并且检测中的干扰因素多，因此开发简便、高效的样品制备与前处理方法，以及具有高灵敏度和选择性的检测方法是十分必要和紧迫的。 本文共分三部分：第一章为相关工作的背景及文献综述；第二章为动物组织中盐酸克伦特罗的气相色谱检测方法的研究及应用；第三、四、五章分别采用不同的检测方法测定动物组织中游离棉酚的含量。具体内容为：第一章概述了动物性食品中兽药残留分析方法的进展，主要介绍了超声波辅助提取、固相萃取、基质固相分散技术和超临界流体萃取等样品前处理技术以及这些方法在兽药残留分析中的应用，并对气相色谱、高效液相色谱和免疫分析法等常用检测方法做了简要概述，最后阐述了本研究工作的目的和意义。第二章建立了气相色谱法直接测定动物组织中盐酸克伦特罗残留量的分析方法。用稀盐酸做提取液，经超声波辅助从动物组织中提取盐酸克伦特罗，再通过C18固相萃取小柱净化及BSTFA衍生化处理样品。最后采用PTE-5毛细管柱分离，电子捕获检测器检测。方法的最低检测限为1.0μg/kg，通过分析方法学评价该方法测定结果准确可靠，可以作为动物组织中盐酸克伦特罗的筛选性检测方法。最后将本方法应用于乌鲁木齐市及周边地区动物性食品中盐酸克伦特罗残留量的调查研究报告中，取得了满意的结果。第三章提出了用高效液相色谱测定动物组织中游离棉酚含量的方法。用70%丙酮水溶液为提取液，经旋转蒸发浓缩样品。最后以BDS HYPERSIL C18<WP=3>（250×4.6mm i.d.5μm）柱为分离柱，二极管阵列检测器检测，外标法定量。方法的最低检出限为0.1mg/kg，回收率为81.4%~101.8%，相对标准偏差为1.6%~10.5%，测定结果符合残留分析要求。第四章初步研究了采用柱前衍生化的高效液相色谱法测定动物组织中游离棉酚的含量。将样品提取与衍生化处理相结合，在待测组分的分子结构上构建强的紫外吸收基团，增加检测器的灵敏度。经样品添加回收实验计算，该方法回收率为60~76%，相对标准偏差为8.2~14.5%，最低检测限为0.02mg/kg，测定结果令人满意。第五章提出了一种用液相色谱/质谱联用仪确证性检测动物组织中游离棉酚的方法。样品经脱水处理后，提取和净化步骤同第三章相似。质谱采用电喷雾离子源，负离子模式检测，选择离子检测质荷比为517。方法检测限为0.5μg/L，平均回收率达79.7%，相对标准偏差为2.2~16.2%，测定结果符合国际食品法典委员会的痕量分析要求。更多还原

【Abstract】 The veterinary drug residues in food has become a weighty and disputed problem in recent years since it is close to public health and has greatly affected the economic benefits of the animal husbandry. The residue level of the veterinary drug residues is nearly 1 μg ~1mg in the food or lower, and there are many interference factors while measuring, so it is extremely necessary and urgent to develop convenient and high-efficient previous treatment method , and the high sensitivity and alternative detection method.This dissertation consists of three parts. The first chapter summarized the progress of veterinary drug residues analysis in animal tissue. Chapter two is the study and application of GC method by which analyzes Clenbuterol(CL) in the animal tissue. The third, four, five chapters adopt different detection methods for determining free gossypol in animal sample respectively. The details are as following:The first chapter mainly introduces some commonly used sample preparation methods and their applications in the analysis of veterinary drug residues. These methods include Sonication-assisted Extraction(SAE), Solid Phase Extraction(SPE), Matrix solid-phase dispersion(MSPD), Supercritical Fluid Extraction(SFE).The regulatory analysis methods such as gas chromatography(GC), high performance liquid chromatography(HPLC) and immunoanalysis(IA) are briefly summarized and the purpose and meaning of the research in this paper are given finally.Chapter 2 describes an analytical method for CL in animal tissues by GC with electron capture detector(ECD) directly. The CL was extracted with hydrochloric <WP=5>acid and purified by C18 SPE column packed, then derivatization with BSTFA. At last CL was carried out by capillary gas chromatography with GC-ECD. The minimum detectable quantity is 1.0 μg/kg. The result is accurate proved by the analytical methodology and can be regarded as screening detection method for Clenbuterol in animal tissues.Finally, we applied this method to survey report which was about CL residues of animal tissues in Urumqi and surrounding area, and got satisfying results.In the third chapter, a method for analysis of Free Gossypol(FG) in animal tissues by HPLC with diode array detector(DAD) was proposed. FG was extracted with a mixture of acetone and water(70:30,v/v) and was concentrate through rotating the evaporation. The analyses were carried out by BDS HYPERSIL C18 (250*4.6mm i.d.5 μm) column with HPLC-DAD. The method was quantified by an external standard mode. The detection limits of the method was 0.1mg/kg, recovery is in the range of 81.4% ~ 101.8%, the relatively standard deviation(RSD) is 1.6% ~10.5%. The result of test coincided with the request of analyzing drug residues.The fourth chapter reported preliminary study of detecting FG in animal tissues with previous-column derivatization by HPLC. Combining sample extraction with derivatization and building strong UV absorption groups in the structures of onmeasuring molecules so as to increase the sensitivity of the detection. Calculating by sample added and retrieving experiment, the recovery of method is 60.6%, RSD is 8.2~14.5%,the detection limit of the method is 0.02mg/kg, the result is satisfied.In the fifth chapter, a HPLC-MS method is presented for FG in the animal tissue. The steps for FG extraction and purification are similar with those in Chapter 3 after getting rid of the water from the animal tissue. The mass spectrum adopts the electrospray ionization(ESI) as ion source and quantitative detection was carried out <WP=6>using the selected ion monitoring(SIM) mode. Choosing 517as mass charge rate of the ion measure. The detection limit of the method is 0.5 μg/L. The average recovery is 79.7%, RSD is 2.2~16.2%, and the result accorded with the request of the world trace analyst of remaining regulation Committee.更多还原