抗氧化剂乙氧喹啉食品残留量的测定方法研究

发布时间：2018-05-13 16:22

本文选题：乙氧喹啉 + 高效液相色谱　；参考：《重庆医科大学》2013年硕士论文

【摘要】：随着人们对于食品鲜度、储存周期等要求的提高，抗氧化剂作为防止食品中营养物质发生变质、酸败、褪色起着必不可少的作用，乙氧喹啉因具有较强的抗氧化、保鲜、防止酸败的作用，而被广泛应用于食品保鲜、饲料防腐等领域中，但人体摄入过量会损害人体多种组织器官，并有引起“三致”作用的潜在风险，所以，包括我国在内的世界各国以及区域组织对于加入食品中的乙氧喹啉最高限量作了规定。目前，乙氧喹啉残留检测方法主要包括高效液相色谱法，气相色谱法，薄层色谱法，液相色谱-串联质谱法等。这些方法覆盖的基质较少，仅限于水果和肉禽基质中乙氧喹啉的残留量检测，因此，有必要建立适用于各种食品中乙氧基喹的检测以及确证方法，以扩大了基质范围，建立了水果、蔬菜、调味料（辣椒粉）、畜肉、水产品、禽蛋等食品中乙氧喹啉水平的HPLC和GC-MS分析方法，从而满足食品中乙氧基喹的质量检验监管需要。第一部分HPLC-荧光法测定食品中的乙氧喹啉残留量目的：建立了食品中乙氧喹啉的HPLC检测方法。方法：色谱柱：采用Agilent Eclipse XDB-C_(18)（150×4.6mm,5m)；流动相：甲醇和水，梯度洗脱；流速：1.0ml/min；柱温：35℃；进样量：20l；检测器：荧光检测器，激发波长：365nm，发射波长：425nm。结果：食品中乙氧喹啉在0.05～10mg/l之间具有良好的线性（γ2≥0.9992）；检出限（S/N=3）为7.5μg/kg，定量限（S/N=10）为25μg/kg；低、中、高浓度的平均回收率80.5%～95.9%，相对标准偏差为3.1%～11.5%。结论：该方法灵特异性好、敏度高、净化分离良好,能有效地消除复杂基质带来的干扰,本方法实用性强，可操作性好，适用于多种食品中乙氧喹啉残留量的检测。第二部分GC-MS法测定食品中乙氧喹啉残留量目的：建立食品中乙氧喹啉的GC-MS检测方法。方法：色谱柱： DB-5MS毛细管（30m×0.25mm×0.25m）；载气：氦气，纯度≥99.999%；恒流模式，流速：1mL/min；柱温升温程序：60℃保持1min，以20℃/min升至260℃，保持1min；以20℃/min升至280℃，保持5min；接口温度：280℃；进样量：2l；质谱条件：四极杆温度:150℃；离子源温度：230℃；电子能量：70eV；数据采集模式：选择性离子监测（SIM）；选择离子为m/z202,174,217,145. 结果：，，乙氧喹啉浓度在10~1000ng/mL范围内具有良好的线性（γ≥0.9998）；检出限为1.5μg/kg，定量限为5.0μg/kg；低、中、高浓度的平均回收率75.4%～89.0%，相对标准偏差为6.1%～9.8%。结论：本方法准确可靠，选择性高，重现性好，可应用于质量标准要求较高的食品中乙氧喹啉的含量测定及确证。
[Abstract]:With the improvement of food freshness, storage cycle and other requirements, antioxidants play an essential role in preventing the deterioration, rancidity and discoloration of nutrients in food. Ethoxoline has a strong antioxidation, preservation and prevention of rancidity, but it is widely used in the fields of food preservation and feed anticorrosion, but the human body is widely used in the field of food preservation. Excessive intake will damage a variety of tissues and organs, and there is a potential risk of causing "three". Therefore, the highest limit of ethoxoline in food is stipulated in all countries including China and regional organizations.
At present, the methods for the determination of ethoxoline residues include high performance liquid chromatography, gas chromatography, thin layer chromatography, liquid chromatography tandem mass spectrometry, etc. these methods cover less matrix and are limited to the residue of ethoxoline in fruit and meat matrix. Therefore, it is necessary to establish a test for ethoxoquine in all kinds of food. In order to meet the requirements of the quality inspection and supervision of ethoxylin in food, HPLC and GC-MS methods have been established to analyze the level of ethoxoline in foods, such as fruit, vegetables, seasoning (pepper powder), animal meat, aquatic products, eggs and other foods.
Part 1 Determination of ethoxy quinoline residues in foods by HPLC- Fluorimetry
Objective: to establish a HPLC method for the determination of ethoxy quinoline in foods.
Method: chromatographic column: using Agilent Eclipse XDB-C_ (18) (150 x 4.6mm, 5m); mobile phase: methanol and water, gradient elution; flow velocity: 1.0ml/min; column temperature: 35 C; sampling quantity: 20L; detector: fluorescence detector, 365nm, emission wavelength: 425nm.
Results: the ethoxoline in food has a good linearity between 0.05 and 10mg/l (gamma 2 > 0.9992), the detection limit (S/N=3) is 7.5 mu g/kg and the quantitative limit (S/N=10) is 25 mu g/kg; the average recovery rate of low, middle and high concentration is 80.5% to 95.9%, and the relative standard deviation is 3.1% to 11.5%..
Conclusion: this method has good specificity, high sensitivity, good purification and separation, and can effectively eliminate the interference caused by complex matrix. This method is practical and easy to operate. It is suitable for the detection of ethoxoline residues in many kinds of food.
Second part GC-MS determination of ethoxy quinoline residues in foods
Objective: to establish a GC-MS method for the determination of ethoxy quinoline in foods.
Method: column: DB-5MS capillary (30M x 0.25mm x 0.25m); carrier gas: helium gas, purity more than 99.999%; constant current mode, velocity: 1mL/min; column temperature heating program: 60 C to maintain 1min, 20 C /min to 260 C, keep 1min; 20 C /min to 280 centigrade, 5min; interface temperature 280; 2L; mass mass conditions: Four Pole pole temperature: 150 centigrade; ion source temperature: 230 C; electronic energy: 70eV; data acquisition mode: selective ion monitoring (SIM); selected ion as m/z202174217145.
Results: the concentration of ethoxoline has a good linearity in the range of 10~1000ng/mL (gamma > 0.9998); the detection limit is 1.5 mu g/kg and the quantitative limit is 5 mu g/kg; the average recovery rate of low, middle and high concentration is 75.4% ~ 89%, and the relative standard deviation is 6.1% ~ 9.8%.
Conclusion: the method is accurate, reliable, highly selective and reproducible, and can be applied to the determination and confirmation of ethoxy quinoline in foods with high quality standard.

【学位授予单位】：重庆医科大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：R155.5

【参考文献】