鸡蛋中四类兽药的高效液相色谱残留检测方法研究
发布时间：2019-04-09 12:21
【摘要】：本研究建立了鸡蛋中喹诺酮类、磺胺类、酰胺醇类、四环素类的药物残留分析方法。采用简单的传统液液萃取结合固相萃取的方法将鸡蛋样品提取、净化后,经高效液相色谱仪分析,测定了鸡蛋中四类兽药的残留,试验结果如下:1.鸡蛋中喹诺酮类药物残留分析方法的研究建立了鸡蛋中4种喹诺酮类药物残留检测的高效液相色谱法。样品采用磷酸盐提取液提取,正己烷除脂,过PLS柱净化,供高效液相色谱分析测定。结果显示,4种喹诺酮类药物在50 ng/g~1000 ng/g浓度范围内呈现良好的线性相关,检出限和定量限分别为10 ng/g和50 ng/g,在10 ng/g、200 ng/g、500 ng/g三个添加浓度回收率为60.2%~68.2%,日内、日间相对标准偏差均小于6.6%。2.鸡蛋中磺胺类药物残留分析方法的研究建立了鸡蛋中6种磺胺类药物残留检测的高效液相色谱法。提取溶剂为乙酸乙酯,结合超声波辅助提取,真空旋转蒸发后,用流动相溶解残留物,过Oasis MCX固相萃取柱,5%氨化甲醇洗脱,选用C18反相色谱柱进行高效液相色谱分析测定。在选定的色谱条件下,6种磺胺类药物在15 ng/g~1000 ng/g浓度范围内呈现良好的线性相关,检出限为5 ng/g、10 ng/g,定量限为15 ng/g、30 ng/g,在10 ng/g、200 ng/g、500 ng/g三个添加浓度回收率为70.1%~82.5%,日内、日间相对标准偏差均小于5.5%。3.鸡蛋中酰胺醇类药物残留分析方法的研究建立了鸡蛋中2种酰胺醇类药物残留检测的高效液相色谱法。样品采用(85+15)乙腈-水溶液提取,正己烷除脂后,再加入乙酸乙酯,真空减压蒸干后,用(5+95)乙腈-水溶液溶解残留物,过C18固相萃取柱,供高效液相色谱测定。研究结果显示,2种酰胺醇类药物在50 ng/g~1000 ng/g浓度范围内呈现良好的线性相关,检出限与定量限分别为10 ng/g和50 ng/g,在10 ng/g、200 ng/g、500 ng/g三个添加浓度回收率为60.6%~71.1%,日内、日间相对标准偏差小于6.5%。4.鸡蛋中四环素类药物残留分析方法的研究建立了鸡蛋中4种四环素类药物残留检测的高效液相色谱法。采用Na2EDTA-Mcllvaine溶液为提取溶剂,PLS固相萃取柱净化,草酸甲醇洗脱,35℃水浴氮气浓缩并定容后,高效液相色谱测定。结果显示,4种四环素类药物在30 ng/g~1000 ng/g浓度范围内线性关系良好,检出限为10 ng/g,定量限为30 ng/g、50 ng/g,在10 ng/g、200 ng/g、500 ng/g三个添加浓度回收率为61.5%~74.4%,日内、日间相对标准偏差小于5.6%。本论文开展了鸡蛋中4类兽药残留分析方法的研究。根据药物的理化特性和鸡蛋基质的特点,优化了各类药物残留检测的样品前处理方法与色谱条件参数,在准确度、灵敏度、特异性、可操作性等方面均获得了较好的效果,能够满足鸡蛋中4类药物残留的检测的相关要求。
[Abstract]:A method for the determination of quinolones, sulfonamides, amides and tetracyclines in eggs was established. The egg samples were extracted by simple liquid-liquid extraction combined with solid phase extraction. After purification, the residues of four kinds of veterinary drugs in eggs were determined by high performance liquid chromatography (HPLC). The results were as follows: 1. Determination of four quinolones residues in eggs by HPLC. The sample was extracted by phosphate extract, removed by n-hexane, purified by PLS column and analyzed by high performance liquid chromatography (HPLC). The results showed that there was a good linear correlation between the four quinolones in the concentration range of 50 ng/g~1000 ng/g, and the detection limits and quantitative limits were 10 ng/g and 50 ng/g, at 10 ng/g,200 ng/g, respectively. The recoveries of the three concentrations of 500 ng/g were 60.2% / 68.2% and within the day, the relative standard deviations (RSD) were all less than 6.6%. A HPLC method for the determination of 6 sulfonamides residues in eggs was established. The solvent was ethyl acetate, combined with ultrasonic assisted extraction. After vacuum rotary evaporation, the residue was dissolved in mobile phase, followed by Oasis MCX solid phase extraction column and eluted with 5% ammoniated methanol. The C 18 reversed phase column was used for high performance liquid chromatography (HPLC) determination. Under the selected chromatographic conditions, 6 sulfonamides showed good linear correlation in the concentration range of 15 ng/g~1000 ng/g, the detection limit was 5 ng/g,10 ng/g, and the detection limit was 15 ng/g,30 ng/g, in 10 ng/g,. The recoveries of the three concentrations of 200 ng/g,500 ng/g were 70.1% / 82.5% and within the day, the relative standard deviations (RSD) were all less than 5.5%. Study on Analysis method of Amido Alcohol residues in Egg A HPLC method was established for the determination of two amides alcohols residues in eggs. The sample was extracted with (8515) acetonitrile-aqueous solution, removed by n-hexane, and then evaporated with ethyl acetate. The residue was dissolved in (595) acetonitrile-aqueous solution and the residue was extracted by C _ (18) solid phase extraction column for determination by high performance liquid chromatography (HPLC). The results showed that there was a good linear correlation between the two amides in the concentration range of 50 ng/g~1000 ng/g, and the detection limits and quantitative limits were 10 ng/g and 50 ng/g, at 10 ng/g,200 ng/g, respectively. The recovery of 500 ng/g was 60.6% and 71.1% respectively. Within day, the relative standard deviation was less than 6.5%. Determination of tetracycline residues in eggs A HPLC method was developed for the determination of tetracycline residues in eggs. Na2EDTA-Mcllvaine solution was used as extraction solvent, purified by PLS solid-phase extraction column, eluted with methanol oxalate, concentrated with nitrogen in water bath at 35 鈩，
本文编号：2455180
[Abstract]:A method for the determination of quinolones, sulfonamides, amides and tetracyclines in eggs was established. The egg samples were extracted by simple liquid-liquid extraction combined with solid phase extraction. After purification, the residues of four kinds of veterinary drugs in eggs were determined by high performance liquid chromatography (HPLC). The results were as follows: 1. Determination of four quinolones residues in eggs by HPLC. The sample was extracted by phosphate extract, removed by n-hexane, purified by PLS column and analyzed by high performance liquid chromatography (HPLC). The results showed that there was a good linear correlation between the four quinolones in the concentration range of 50 ng/g~1000 ng/g, and the detection limits and quantitative limits were 10 ng/g and 50 ng/g, at 10 ng/g,200 ng/g, respectively. The recoveries of the three concentrations of 500 ng/g were 60.2% / 68.2% and within the day, the relative standard deviations (RSD) were all less than 6.6%. A HPLC method for the determination of 6 sulfonamides residues in eggs was established. The solvent was ethyl acetate, combined with ultrasonic assisted extraction. After vacuum rotary evaporation, the residue was dissolved in mobile phase, followed by Oasis MCX solid phase extraction column and eluted with 5% ammoniated methanol. The C 18 reversed phase column was used for high performance liquid chromatography (HPLC) determination. Under the selected chromatographic conditions, 6 sulfonamides showed good linear correlation in the concentration range of 15 ng/g~1000 ng/g, the detection limit was 5 ng/g,10 ng/g, and the detection limit was 15 ng/g,30 ng/g, in 10 ng/g,. The recoveries of the three concentrations of 200 ng/g,500 ng/g were 70.1% / 82.5% and within the day, the relative standard deviations (RSD) were all less than 5.5%. Study on Analysis method of Amido Alcohol residues in Egg A HPLC method was established for the determination of two amides alcohols residues in eggs. The sample was extracted with (8515) acetonitrile-aqueous solution, removed by n-hexane, and then evaporated with ethyl acetate. The residue was dissolved in (595) acetonitrile-aqueous solution and the residue was extracted by C _ (18) solid phase extraction column for determination by high performance liquid chromatography (HPLC). The results showed that there was a good linear correlation between the two amides in the concentration range of 50 ng/g~1000 ng/g, and the detection limits and quantitative limits were 10 ng/g and 50 ng/g, at 10 ng/g,200 ng/g, respectively. The recovery of 500 ng/g was 60.6% and 71.1% respectively. Within day, the relative standard deviation was less than 6.5%. Determination of tetracycline residues in eggs A HPLC method was developed for the determination of tetracycline residues in eggs. Na2EDTA-Mcllvaine solution was used as extraction solvent, purified by PLS solid-phase extraction column, eluted with methanol oxalate, concentrated with nitrogen in water bath at 35 鈩，
本文编号：2455180
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