超高效液相色谱法测定牛奶及奶制品中四环素类药物残留
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摘要
采用超高效液相色谱法对牛奶及奶制品中四环素类药物残留进行同时检测,着重研究样品的前处理,最终确立乙腈/水(体积比为4∶1)为提取剂,无水乙醇为沉淀剂,并采用氨基柱作为净化柱。结果表明:四环素类药物线性关系良好,RSD<5%,实际样品检出率为100%,超标率在13.33%～60.00%之间。此方法灵敏度高、操作快速、简便,回收率在89.75%～92.26%。
Ultra-high performance liquid chromatography was used to detect tetracycline drug residues in milk and dairy products at the same time,focusing on the pre-treatment of samples,and finally establishing acetonitrile/water(volume ratio 4 ∶1) as an extractant and anhydrous ethanol as a precipitator,the amino column was used as a purification column. A precipitant and an amino column was used as a purification column. The results showed that the linear relationship of tetracyclines was good,RSD<5 %,the actual sample detection rate was 100 %,and the over-standard rate was between 13.33 % and 60.00 %. The method had high sensitivity,fast and simple operation,and the recovery rate was from 89.75 % to 92.26 %.
Ultra-high performance liquid chromatography was used to detect tetracycline drug residues in milk and dairy products at the same time,focusing on the pre-treatment of samples,and finally establishing acetonitrile/water(volume ratio 4 ∶1) as an extractant and anhydrous ethanol as a precipitator,the amino column was used as a purification column. A precipitant and an amino column was used as a purification column. The results showed that the linear relationship of tetracyclines was good,RSD<5 %,the actual sample detection rate was 100 %,and the over-standard rate was between 13.33 % and 60.00 %. The method had high sensitivity,fast and simple operation,and the recovery rate was from 89.75 % to 92.26 %.
引文
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[4]江秀红.液相色谱-串联质谱法测定鸭肉中四环素类药物残留[J].福建畜牧兽医,2015,37(4):1-3
[5]宓捷波,许迪明,李淑静,等.奶粉中残留兽药的Qu ECh ERS方法应用研究[J].食品研究与开发,2015,36(2):121-125
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[11]江羚,曾昆,邵杰,等.四环素类抗生素快速分析方法研究进展[J].江苏农业科学,2018,48(8):15-21
[12]庞小莲,刘吉成,黎美莲,等.超高效液相色谱-串联质谱法测定畜禽肉及其内脏中四环素类兽药残留量[J].食品安全质量检测学报,2018,9(15):4089-4098
[13]王敏娟,胡佳薇,田丽,等.超高效液相色谱-串联质谱法同时测定鸡蛋中21种喹诺酮及四环素类抗生素残留[J].食品研究与开发,2017,21(4):473-476
[14]梅英杰,史新宇,董瑾,等.超高效液相色谱-串联质谱法同时检测鸡肉中氯霉素、四环素、金霉素和土霉素[J].食品与发酵工业,2017,43(8):240-245
[15]刘洋,张乐.UPLC法测定水产品中土霉素、四环素和金霉素残留量研究[J].杭州农业与科技,2015(1):31-33
[16]黄闯,孙芝杨,李新建,等.牛奶中四环素类兽残的快速检测关键技术应用研究[J].食品研究与开发,2017,38(10):134-138
[17]唐宁莉,范晶晶,马小龙,等.共振散射光谱法测定牛奶中的四环素[J].食品研究与开发,2018,19(38):134-138
[18]Danlian Huang,Xigui Liu,Cuilai,et al.Recent advances in sensors for tetracycline antibiotics and their applications[J].Trends in Analytical,2018,10(9):260-274
[19]高志莹,刘琦,洪霞,等.LC-MS/MS测定牛奶中氯霉素和四环素类抗生素[J].食品工业,2016,37(10):287-290
[20]Korkmaz,Kuplulu,Cil.et al.Detection of sulfonamide and tetracycline antibiotic residues in Turkish pine honey[J].I nternational Journal of Food Properties,2017,34(4):50-55
[2]葛云芝,于小波,周光宏,等.高效液相色谱法同时测定鸡肉中3种四环素类抗生素残留[J].食品科学,2013,34(10):180-183
[3]朱晓华,刘畅,吴光红.液相色谱法测定鱼肉中土霉素残留前处理方法的改进[J].中国兽药杂志,2010,44(5):4-8
[4]江秀红.液相色谱-串联质谱法测定鸭肉中四环素类药物残留[J].福建畜牧兽医,2015,37(4):1-3
[5]宓捷波,许迪明,李淑静,等.奶粉中残留兽药的Qu ECh ERS方法应用研究[J].食品研究与开发,2015,36(2):121-125
[6]高广慧,李阳,孙晓娟,等.HPLC法测定牛羊肉中土霉素、四环素、金霉素残留量[J].食品研究与开发,2013,34(16):94-96
[7]吴海霞,徐红颖,马光路.牛、羊、猪、鸡肉中土霉素残留量的检测分析[J].黑龙江畜牧兽医,2016(11上):287-288
[8]邢俊生,张彬,李倩.食品虾仁中土霉素、四环素、金霉素含量测定方法的建立[J].中国药事,2017,31(10):1199-1203
[9]梁金玲,黄玉霞,何金兴.分子印迹固相萃取-高效液相色谱法检测鸡肉中的四环素类抗生素残留[J].现代食品科技,2018,34(7):224-229
[10]栗慧,李佳仪,彭伟.四环素类抗生素检测方法研究进展[J].河北北方学院学报,2018,34(2):41-48
[11]江羚,曾昆,邵杰,等.四环素类抗生素快速分析方法研究进展[J].江苏农业科学,2018,48(8):15-21
[12]庞小莲,刘吉成,黎美莲,等.超高效液相色谱-串联质谱法测定畜禽肉及其内脏中四环素类兽药残留量[J].食品安全质量检测学报,2018,9(15):4089-4098
[13]王敏娟,胡佳薇,田丽,等.超高效液相色谱-串联质谱法同时测定鸡蛋中21种喹诺酮及四环素类抗生素残留[J].食品研究与开发,2017,21(4):473-476
[14]梅英杰,史新宇,董瑾,等.超高效液相色谱-串联质谱法同时检测鸡肉中氯霉素、四环素、金霉素和土霉素[J].食品与发酵工业,2017,43(8):240-245
[15]刘洋,张乐.UPLC法测定水产品中土霉素、四环素和金霉素残留量研究[J].杭州农业与科技,2015(1):31-33
[16]黄闯,孙芝杨,李新建,等.牛奶中四环素类兽残的快速检测关键技术应用研究[J].食品研究与开发,2017,38(10):134-138
[17]唐宁莉,范晶晶,马小龙,等.共振散射光谱法测定牛奶中的四环素[J].食品研究与开发,2018,19(38):134-138
[18]Danlian Huang,Xigui Liu,Cuilai,et al.Recent advances in sensors for tetracycline antibiotics and their applications[J].Trends in Analytical,2018,10(9):260-274
[19]高志莹,刘琦,洪霞,等.LC-MS/MS测定牛奶中氯霉素和四环素类抗生素[J].食品工业,2016,37(10):287-290
[20]Korkmaz,Kuplulu,Cil.et al.Detection of sulfonamide and tetracycline antibiotic residues in Turkish pine honey[J].I nternational Journal of Food Properties,2017,34(4):50-55