【作者】 朱宽正；

【导师】 梅素容；

【作者基本信息】 华中科技大学 ， 环境科学， 2007， 硕士

【摘要】 对复杂基质中痕量成分的多残留组分分析和确证分析已成为食品安全分析的重大难题。传统的仪器检测方法对这一问题难以解决,如气相色谱法（GC）、液相色谱法（LC）、气相色谱质谱法（GC-MS）等。液相色谱-串联质谱联用技术（LC-MS/MS）结合了液相色谱、串联质谱两者的优点,不仅分离能力强,选择性好,灵敏度高,而且还可以对复杂基质样品中的痕量成分进行确证分析,已成为食品安全分析手段中必不可少的组成部分。本论文主要内容如下:（1）本文对食品安全问题和食品分析的现状进行了概述,并对液相色谱-串联质谱联用技术的基本原理和发展以及其在食品分析中的应用进行了综述。（2）采用液相色谱-串联质谱法（LC-MS/MS）进行了水产品中三苯甲烷类药物的残留分析研究。同时测定了水产品中的孔雀石绿、结晶紫以及它们的隐色代谢物残留。将匀质后的水产品样品,用乙腈和乙酸铵缓冲液提取,合并提取液,用二氯甲烷反提取,经中性氧化铝柱和PRS柱固相萃取净化,没有使用氧化铅柱在线氧化,色谱分离后直接进入串联质谱检测器。采用电喷雾正离子,多反应检测（MRM）模式检测。方法的检测限可达0.5ng/g,添加样品平均回收率为77.6%～98.1%,相对标准偏差均小于8.2%。（3）采用液相色谱-串联质谱法（LC-MS/MS）同时测定了蜂王浆中氯霉素,甲砜霉素和氟甲砜霉素残留。样品加入阴性蜂蜜和水均质后,采用乙酸乙酯提取,蒸发浓缩,C₁₈固相萃取净化。HPLC分离后,串联质谱法以电喷雾负离子多反应监测方式（MRM）进行定性定量分析。通过对固相萃取条件的优化,大大减小了基质的干扰。氯霉素,氟甲砜霉素和甲砜霉素的检出限分别为0.1ng/g,0.2ng/g和0.5ng/g,平均回收率为79.9%～88.4%,相对标准偏差（RSD）均小于8.2%。更多还原

【Abstract】 Confirmatory multiresidue analysis for organic compounds at trace levels in complex matrixes is required in food analysis. Conventional techniques in food analysis, such as Gas chromatography （GC）, Liquid chromatography （LC）, Gas chromatography mass spectrometry （GC-MS）, etc., can’t meet the demands. Liquid chromatography tandem mass spectrometry （LC-MS/MS） technique frequently provides specific, selective and sensitive quantitative results, and allows unequivocal identification of traces of contaminants in complex food matrices, which has become one of the major tools in food analysis.The main contents in this thesis are described as follows:（1）The paper reviews the importance of food safety and the status of food analysis, and introduces the basic principle, characteristics of LC-MS/MS and its application in food analysis.（2）A liquid chromatography tandem mass spectrometry （LC-MS/MS） method was described for Simultaneous determination of residues of malachite green （MG）,leucomalachite green（LMG）,rystal violet（CV）and leucocrystal violet（LCV） in aquatic products. The targeted analytes were extracted from homogenized samples with a mixture of acetonitrile and ammonium acetate buffer, partitioned against methylene chloride, and purified on tandem neutral alumina and PRS SPE cartridges. Chromatographic Separation was achieved by using ZORBAX SB-C18 column with an isocratic mobile phase consisting of ammonium acetate （0.05mM） and acetonitrile（10/90,V/V）without the need for in-line post-column oxidation with PbO₂. Identification and quantification were performed using multiple reaction monitoring （MRM） with one precursor ion and two product ions for each analyte and electrospray ionization in positive mode. Limits of detection were 0.5ng/g. Recoveries were in the range of 77.6%～98.1%, and the RSDs were less than 8.2%.（3）A method was presented for simultaneous determination residues of Chloramphenicol （CAP）,Thiamphenicol （TAP） and Florfenicol （FF） in royal jelly by using high performance liquid chromatography tandem mass spectrometry （LC–MS/MS）.After a preliminary homogenization in negative honey and water, samples were extracted with ethyl acetate, and evaporated to dryness; the following clean up was carried out on a C18 SPE cartridge. After reversed-phase HPLC separation, identification and quantification were performed using multiple reaction monitoring （MRM） and electrospray ionization in negative mode. In order to dispel the matrix interference, the conditions of solid phase extraction were optimized. The detection limits of the method were 0.1ng/g,0.2ng/g and 0.5ng/g for CAP, FF and TAP, respectively. The average recoveries were 79.9%⁸8.4%, and the RSD were lower than 8.2.%.更多还原