摘要
随着人们环保意识的提高,越来越多的食品安全事件引起人们的关注,如奶粉中三聚氰胺超标事件,红牛检出可卡因等,这些事件不仅给人民生命财产带来巨大损失,还带来了极其恶劣的社会影响和严重的环境污染问题。因此如何采取有效地检测方法对食品中残留污染物质进行检测就成了当务之急。
环境中残留抗生素不仅会对周围环境造成严重污染,还会给人体健康造成危害,因此,就有必要对环境中残留抗生素进行处理。现有的残留抗生素检测方法存在灵敏度低、选择范围较单一、准确性较差等缺点。研究一种分析快速、操作简便、准确的检测微痕量抗生素的方法是当务之急。
离子液体是完全由有机阳离子和无机或有机阴离子构成的在室温或者室温附近温度(-30℃～50℃)下呈液态的物质。由于离子液体特有的性质使得对其的研究越来越受到人们的关注。离子液体可应用于很多方面,其应用范围包括电池电解、合成工业的溶剂、萃取等。
本文采用两步法合成了四种不同的离子液体,一步法合成了两种不同的疏水性离子液体,并采用紫外光谱、核磁共振和红外光谱对离子液体结构进行表征；以合成的离子液体为萃取剂,对红霉素进行萃取,研究了他们对红霉素的萃取、分离效果,考察了不同因素对萃取率的影响,还对比了离子液体和传统有机溶剂对红霉素的萃取率,对离子液体进行再生处理。
最佳实验条件为：
[Bmim]PF6:离子液体加入量为每份2.00g,即71g/mL,温度为323.15K,振荡时间为2.0h,pH值为5,干扰物质的存在对萃取率的影响不大,离子液体可重复使用不超过5次；
[Omim]BF4:离子液体加入量为每份2.50g,即89g/mL,温度为323.15K,振荡时间为1.5h,pH值为8,干扰物质的存在对萃取率的影响不大,离子液体可重复使用不超过5次；
[Emim]BF4/ NaH2PO4双水相体系：离子液体加入量为每份3.50g,即125g/mL,固体NaH2PO4的加入量为20.0g,即浓度为39.0%。温度为303.15K,振荡时间为2h～2.5h,pH值为6,离子液体可重复使用不超过5次；
[Bmim]BF4/ NaH2PO4双水相体系：离子液体加入量为每份1.50g,即54g/mL,固体NaH2PO4的加入量为11.0g,即浓度为27.0%。温度为313.15K,振荡时间为2.0h,pH值为7,离子液体可重复使用不超过5次。
离子液体经处理后可继续使用。
利用实验结果萃取鸡蛋中残留的微痕量红霉素,并建立离子液体富集、分离环境中残留的微痕量红霉素的检测方法。
离子液体可以富集残留的痕量红霉素,并能萃取红霉素。[Bmim]PF6的线性方程为A=13.6C-0.60,相关系数为0.9982,线性范围为0.5～100μg/mL,检出限为4μg/kg,[Omim]BF4线性方程为A=6.42C-0.035,相关系数为0.9420,线性范围为0.5～100μg/mL,检出限为5μg/kg。
样品的红霉素加标回收率为87.5～108.3%。
结果表明,离子液体对红霉素有良好的萃取效果。
With the environmental awareness improvement, more and more food safety incidents cause people's concern. For example milk exceedingmelamine incident, toro detected cocaine, etc. These accidents lead to loss of life and property, social influences and serious environmental pollution accidents. How to take effective detection methods to detection trace residue pollutants in food is urgent.
The trace residue pollutants in environment can caused around environment serious pollutions, and hazard health to people. So we must to deal with the trace residue pollutants in environment. Now effective detection methods to trace residue pollutants have shortcomings, for example low sensitivity, choice range single, accuracy poor, etc. So, develope detection methods with analysis fast, operation simple and accuracy is urgent
Ionic liquid is liquid materials totally formed by organic cation and organic anion or inorganic ionic under the room temperature or the nearby temperature (-30℃～50℃). Ionic liquids (ILs), considered to be a relatively recent magical chemical due to their unique properties, have a large variety of applications in all areas of the chemical industries. The areas of application include electrolyte in batteries, plasticizers, solvents in synthesis, extraction, etc.
In the article, two-step method synthetic four difference ionic liquids, one-step method synthetic two difference hydrophobic ionic liquids, and take UV, NMR, and IR identified ionic liquids. Take synthetical ionic liquids as extractant to extract erythromycin. Research effect of extraction, separation. Study extracted methods, the numbers of ionic liquids, initial concentration of erythromycin, temperature, the effects of pH value, oscillation time, kinds of salts, reused to the influence to the extraction rate. Compared ionic liquids to traditional organic solvents in the extraction rate. Deal with the regeneration of ionic liquids.
The best experiment condition:
[Bmim]PF6:the dosage of IL is 2.00g, that 71g/mL, temperature is 323.15K, oscillation time is 2.0h, pH value is 9, the existence of interfering substance is not effect extraction rate. IL can reuse 5 times.
[Omim]BF4:the dosage of IL is 1.00g, that 89g/mL, temperature is 323.15K, oscillation time is 1.5h, pH value is 8, the existence of interfering substance is not effect extraction rate. IL can reuse 5 times.
[Emim]BF4/ NaH2PO4: the dosage of IL is 3.50g, that 125g/mL, the dosage of Sodium dihydrogen phosphate is 20.0g, that concentration is 39%, temperature is 303.15K, oscillation time is 2.0h～2.5h, pH value is 6, the existence of interfering substance is not effect extraction rate. IL can reuse 5 times.
[Bmim]BF4/ NaH2PO4: the dosage of IL is 1.50g, that 54g/mL, the dosage of Sodium dihydrogen phosphate is 11.0g, that concentration is 27%, temperature is 313.15K, oscillation time is 2.0h, pH value is 7, the existence of interfering substance is not effect extraction rate. IL can reuse 5 times.
Take the results to extract the trace residue erythromycin in eggs. And establish method that take ionic liquids to enrichment and separate the trace residue erythromycin in environment.
[Bmim]PF6's linear equation is A=13.6C-0.60, correlation coefficient is 0.9982, linear range is 0.5～100μg/mL, detection limit is 4μg/kg, [Omim]BF4's linear equation is A=6.42C-0.035, correlation coefficient is 0.9420, linear range is 0.5～100μg/mL, detection limit is 5μg/kg.The recovery rate of erythromycin in sample is 87.5～108.3%.
The results show that ionic liquids have better extraction rate to erythromycin.
引文
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