【作者】 杨玉霞；

【导师】 凌敏； 甘宾宾；

【作者基本信息】 广西大学 ， 分析化学， 2007， 硕士

【摘要】 现今食品安全，尤其是进出口食品的安全问题，越来越受到各国政府的关注，政府相继出台大量文件，对食品中添加物的种类限定越来越多，限量标准也越来越高，食品中违禁添加物的检出及合法添加物的超量问题已成为主要的食品不安全因素，也成为食品分离分析的热点问题。本文采用高效液相色谱仪—光电二极管阵列检测器（HPLC-PDAD）作为检测手段，对食品中有害的色剂苏丹红和四种四环素类抗生素的定性定量的分析方法进行了较系统的研究，根据HPLC-PDAD方法的特点，能够以保留时间和特征紫外可见吸收光谱作为定性、定量的依据，保证了的分离分析方法的可靠性。1、建立了高效液相色谱—光电二极管阵列检测器（HPLC-PDAD）快速测定食品中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ。实验采用聚酰胺粉净化样品提取液，色谱柱为ZORBAX SB-C₁₈柱，以甲醇为流动相，流速1.0 mL／min。苏丹红在1～150 ng范围内呈良好线性，相关系数为0.99992～0.99997；检出限为0.1 ng（3倍信噪比）；回收率在94.8％～97.2％之间。该方法有效地去除了样品中的杂质干扰，如合成色素、辣椒素、番茄素、红曲米等，操作简便，可作为食品中苏丹红快速、准确的检测方法。2、运用该方法对市场上抽查的79份样品进行了分析检测，检测8份含苏丹红Ⅰ的阳性样品，其余的样品均未检出苏丹红Ⅰ，其检出率10.12％。并对含苏丹红Ⅰ的阳性样品运用了气—质（GC-MS）进行了确证。3、建立了可同时检测四环素、土霉素、金霉素和多西环素的固相萃取（SPE）—高效液相色谱（HPLC）—光电二极管阵列检测器（PDAD）方法。色谱条件为：色谱柱：AICHROM^TM C₁₈，（4.6×250 nm，5μm）；流动相：乙腈：甲醇：0.01 mol／L草酸的水溶液（体积比为20：10：70）；流速：1.0 mL／min；进样量：10μL；柱温：30℃；检测波长：365 nm。优化了样品的前处理条件：向组织样品中加入三氯乙酸作沉淀剂，匀浆震荡后；分别用15 mL、15 mL、10 mL的Na₂EDTA-Mcllvaine缓冲溶液进行超声波提取，每次20 min，合并三次上清液以4000 r／min离心10 min，上清液运用Oasis HLB固相萃取柱进行净化。有效地提高了样品的提取效率。4、运用以上色谱条件和样品前处理条件对肉类和蜂蜜等不同食品样品进行回收率、准确度和精密度测定及样品实测，回收率在81.2％以上，变异系数小于5.01％，相关系数为0.9991～0.9999；土霉素、四环素、金霉素和多西环素的检出限（3倍信噪比）分别为0.034 mg／kg，0.018 mg／kg，0.024 mg／kg和0.050 mg／kg；结果表明方法操作简便，适于食品中痕量物质的分析。更多还原

【Abstract】 The separation and analysis of harmful food additive residues is a hot topicin the organic contamination analysis. At present, a number of methods dealingwith the separation and analysis of harmful food additive residues have beendeveloped. This thesis concerns about analytical approach development ofSudan dyes and Tetracyclines.In this study, HPLC-PDAD was applied to analysis tetracyclines and Sudandyes. PDAD is a good detector for quantitative analysis of known substance forqualitative analysis of unknown samples. In this study, it can be got PDADChromatogram and Spectrogram in single analysis. By the analytical information, reliable result can be drawn.Firstly, a method has been developed for the rapid determination of SudanⅠ、Ⅱ、Ⅲ、Ⅳin food by high performance liquid chromatography. The Sudandyes were purified using polyamide and separated on a ZORBAX SB-C₁₈column with methanol as the mobile phase and detected with HPLC-PDAD. Theflow-rate was 1.0 ml/min. The calibration curve of each Sudan dyes showedgood linearity in the range of 1～150 ng （r=0.99992～0.99997）.The detection limits of each Sudan dyes was 0.1 ng.The recovery rate was 94.8％～97.2％. Thismethod is simple, rapid, accurate and reliable.Secondly, a high performance liquid chromatography method has beenestablished for determination of Tetracycline（TC）, Oxtetracycline（OTC）,Chlortetracycline（CTC） and Doxyeycline（DC） in a test. Tetracyclines weresuccessfully separated on an AICHROM^TM C₁₈, （4.6×250 nm, 5μm）, usingAcetonitrile: Methanol: 0.01 mol/L Oxalic acid （20:10:70, volume ratio） asmobile phase at a flow rate of 1.0 mL/min, detected by photo diode arraydetector at 365 nm, under 30℃, injecting 10μL each time.Thirdly, the tetrcyclines were extracted into a buffer solution, to provide forthe sample enrichment and clean up, then were cleaned up by Oasis HLB SPE.Recoveries exceeded 80.12％for all tetracyclines at all levels. Correlationcoefficients of standards curves for TC, OTC, CTC and DC ranged from 0.9991to 0.9999. The limits of detection of the method were all below 0.05 mg/kg,it can be applied to routine surveillance programs.Detecting different foods such as pig meat, chicken and honey by thismethod. The recoveries are between 81.2％～95.8％and the RSD is between6.28％～0.89％. The procedure is rapid, precise, and requires minimal preparationand organic solvents, The results show that this method is accurate, rapid andsimple, suitable for micro analysis in food.更多还原