雞蛋中四類獸藥的高效液相色譜殘留檢測(cè)方法研究
發(fā)布時(shí)間：2019-04-09 12:21
【摘要】：本研究建立了雞蛋中喹諾酮類、磺胺類、酰胺醇類、四環(huán)素類的藥物殘留分析方法。采用簡(jiǎn)單的傳統(tǒng)液液萃取結(jié)合固相萃取的方法將雞蛋樣品提取、凈化后,經(jīng)高效液相色譜儀分析,測(cè)定了雞蛋中四類獸藥的殘留,試驗(yàn)結(jié)果如下:1.雞蛋中喹諾酮類藥物殘留分析方法的研究建立了雞蛋中4種喹諾酮類藥物殘留檢測(cè)的高效液相色譜法。樣品采用磷酸鹽提取液提取,正己烷除脂,過PLS柱凈化,供高效液相色譜分析測(cè)定。結(jié)果顯示,4種喹諾酮類藥物在50 ng/g~1000 ng/g濃度范圍內(nèi)呈現(xiàn)良好的線性相關(guān),檢出限和定量限分別為10 ng/g和50 ng/g,在10 ng/g、200 ng/g、500 ng/g三個(gè)添加濃度回收率為60.2%~68.2%,日內(nèi)、日間相對(duì)標(biāo)準(zhǔn)偏差均小于6.6%。2.雞蛋中磺胺類藥物殘留分析方法的研究建立了雞蛋中6種磺胺類藥物殘留檢測(cè)的高效液相色譜法。提取溶劑為乙酸乙酯,結(jié)合超聲波輔助提取,真空旋轉(zhuǎn)蒸發(fā)后,用流動(dòng)相溶解殘留物,過Oasis MCX固相萃取柱,5%氨化甲醇洗脫,選用C18反相色譜柱進(jìn)行高效液相色譜分析測(cè)定。在選定的色譜條件下,6種磺胺類藥物在15 ng/g~1000 ng/g濃度范圍內(nèi)呈現(xiàn)良好的線性相關(guān),檢出限為5 ng/g、10 ng/g,定量限為15 ng/g、30 ng/g,在10 ng/g、200 ng/g、500 ng/g三個(gè)添加濃度回收率為70.1%~82.5%,日內(nèi)、日間相對(duì)標(biāo)準(zhǔn)偏差均小于5.5%。3.雞蛋中酰胺醇類藥物殘留分析方法的研究建立了雞蛋中2種酰胺醇類藥物殘留檢測(cè)的高效液相色譜法。樣品采用(85+15)乙腈-水溶液提取,正己烷除脂后,再加入乙酸乙酯,真空減壓蒸干后,用(5+95)乙腈-水溶液溶解殘留物,過C18固相萃取柱,供高效液相色譜測(cè)定。研究結(jié)果顯示,2種酰胺醇類藥物在50 ng/g~1000 ng/g濃度范圍內(nèi)呈現(xiàn)良好的線性相關(guān),檢出限與定量限分別為10 ng/g和50 ng/g,在10 ng/g、200 ng/g、500 ng/g三個(gè)添加濃度回收率為60.6%~71.1%,日內(nèi)、日間相對(duì)標(biāo)準(zhǔn)偏差小于6.5%。4.雞蛋中四環(huán)素類藥物殘留分析方法的研究建立了雞蛋中4種四環(huán)素類藥物殘留檢測(cè)的高效液相色譜法。采用Na2EDTA-Mcllvaine溶液為提取溶劑,PLS固相萃取柱凈化,草酸甲醇洗脫,35℃水浴氮?dú)鉂饪s并定容后,高效液相色譜測(cè)定。結(jié)果顯示,4種四環(huán)素類藥物在30 ng/g~1000 ng/g濃度范圍內(nèi)線性關(guān)系良好,檢出限為10 ng/g,定量限為30 ng/g、50 ng/g,在10 ng/g、200 ng/g、500 ng/g三個(gè)添加濃度回收率為61.5%~74.4%,日內(nèi)、日間相對(duì)標(biāo)準(zhǔn)偏差小于5.6%。本論文開展了雞蛋中4類獸藥殘留分析方法的研究。根據(jù)藥物的理化特性和雞蛋基質(zhì)的特點(diǎn),優(yōu)化了各類藥物殘留檢測(cè)的樣品前處理方法與色譜條件參數(shù),在準(zhǔn)確度、靈敏度、特異性、可操作性等方面均獲得了較好的效果,能夠滿足雞蛋中4類藥物殘留的檢測(cè)的相關(guān)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，
本文編號(hào)：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，
本文編號(hào)：2455180
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