本文選題：乙氧喹啉 + 高效液相色譜��； 參考：《重慶醫(yī)科大學(xué)》2013年碩士論文

【摘要】：隨著人們對于食品鮮度、儲存周期等要求的提高，抗氧化劑作為防止食品中營養(yǎng)物質(zhì)發(fā)生變質(zhì)、酸敗、褪色起著必不可少的作用，乙氧喹啉因具有較強(qiáng)的抗氧化、保鮮、防止酸敗的作用，而被廣泛應(yīng)用于食品保鮮、飼料防腐等領(lǐng)域中，但人體攝入過量會損害人體多種組織器官，并有引起“三致”作用的潛在風(fēng)險(xiǎn)，所以，包括我國在內(nèi)的世界各國以及區(qū)域組織對于加入食品中的乙氧喹啉最高限量作了規(guī)定。 目前，乙氧喹啉殘留檢測方法主要包括高效液相色譜法，氣相色譜法，薄層色譜法，液相色譜-串聯(lián)質(zhì)譜法等。這些方法覆蓋的基質(zhì)較少，僅限于水果和肉禽基質(zhì)中乙氧喹啉的殘留量檢測，因此，有必要建立適用于各種食品中乙氧基喹的檢測以及確證方法，以擴(kuò)大了基質(zhì)范圍，建立了水果、蔬菜、調(diào)味料（辣椒粉）、畜肉、水產(chǎn)品、禽蛋等食品中乙氧喹啉水平的HPLC和GC-MS分析方法，從而滿足食品中乙氧基喹的質(zhì)量檢驗(yàn)監(jiān)管需要。 第一部分HPLC-熒光法測定食品中的乙氧喹啉殘留量 目的：建立了食品中乙氧喹啉的HPLC檢測方法。 方法：色譜柱：采用Agilent Eclipse XDB-C_(18)（150×4.6mm,5m)；流動相：甲醇和水，梯度洗脫；流速：1.0ml/min；柱溫：35℃；進(jìn)樣量：20l；檢測器：熒光檢測器，激發(fā)波長：365nm，發(fā)射波長：425nm。 結(jié)果：食品中乙氧喹啉在0.05～10mg/l之間具有良好的線性（γ2≥0.9992）；檢出限（S/N=3）為7.5μg/kg，定量限（S/N=10）為25μg/kg；低、中、高濃度的平均回收率80.5%～95.9%，相對標(biāo)準(zhǔn)偏差為3.1%～11.5%。 結(jié)論：該方法靈特異性好、敏度高、凈化分離良好,能有效地消除復(fù)雜基質(zhì)帶來的干擾,本方法實(shí)用性強(qiáng)，可操作性好，適用于多種食品中乙氧喹啉殘留量的檢測。 第二部分GC-MS法測定食品中乙氧喹啉殘留量 目的：建立食品中乙氧喹啉的GC-MS檢測方法。 方法：色譜柱： DB-5MS毛細(xì)管（30m×0.25mm×0.25m）；載氣：氦氣，純度≥99.999%；恒流模式，流速：1mL/min；柱溫升溫程序：60℃保持1min，以20℃/min升至260℃，保持1min；以20℃/min升至280℃，保持5min；接口溫度：280℃；進(jìn)樣量：2l；質(zhì)譜條件：四極桿溫度:150℃；離子源溫度：230℃；電子能量：70eV；數(shù)據(jù)采集模式：選擇性離子監(jiān)測（SIM）；選擇離子為m/z202,174,217,145. 結(jié)果：，，乙氧喹啉濃度在10~1000ng/mL范圍內(nèi)具有良好的線性（γ≥0.9998）；檢出限為1.5μg/kg，定量限為5.0μg/kg；低、中、高濃度的平均回收率75.4%～89.0%，相對標(biāo)準(zhǔn)偏差為6.1%～9.8%。 結(jié)論：本方法準(zhǔn)確可靠，選擇性高，重現(xiàn)性好，可應(yīng)用于質(zhì)量標(biāo)準(zhǔn)要求較高的食品中乙氧喹啉的含量測定及確證。
[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.

【學(xué)位授予單位】：重慶醫(yī)科大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2013
【分類號】：R155.5

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