动物源食品中四环素类药物多残留测定的高效液相色谱法研究
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- 英文论文题名：Determination of Tetracylines residues in animal derived food by High Performance Liquid Chromatography
- 论文作者：李慧素 ; 吴宁鹏 ; 彭丽 ; 董晓莹
- 英文论文作者：LI Hui-su ; WU Ning-peng ; PENG Li ; Dong Xiao-ying ; Henan Institute of Veterinary Drug and Feeds Control
- 年：2016
- 作者机构：河南省兽药饲料监察所;
- 论文关键词：四环素类药物 ; 多残留 ; 高效液相色谱法 ; 动物源食品
- 英文论文关键词：Tetracylines ; residues ; HPLC ; animal derived food
- 会议召开时间：2016-09-18
- 会议录名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会论文集
- 语种：中文
- 分类号：S859.84;O657.72
- 学会代码：ZGXJ
- 会议名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会
- 会议地点：中国四川成都
- 主办单位：中国畜牧兽医学会动物药品学分会
- 学会名称：中国畜牧兽医学会
- 页数：10
- 文件大小：1035k
- 原文格式：O
- 会议级别：全国
摘要
优化并建立了10种不同动物源食品中四环素类药物多残留的高效液相色谱检测方法。样品经Na_2EDTA-Mcllvaine缓冲液提取,HLB固相萃取柱和弱酸型阳离子交换柱净化,0.01 mol/L三氟乙酸溶液-乙腈为流动相,350nm为检测波长,外标法定量。四环素类药物在50~5000μg/L的浓度范围内呈线性相关,相关系数均为0.999。方法对四环素类药物在猪、牛、羊、鸡的肝脏、肾脏、猪和鸡的皮+脂肪中的检测限为50μg/kg,定量限为100μg/kg。在100~1200μg/kg添加浓度范围内,土霉素、四环素、金霉素和多西环素的回收率为61.0%~118.5%,批间变异系数为0.4%~14.5%。本方法灵敏度高,重现性好,各项技术指标均满足国内外相关法规要求,可用于动物肝脏、肾脏、脂肪组织中四环素类药物的多残留检测。
A method based on high performance liquid chromatography(HPLC) has been developed for the determination of Tetracylines residues in animal derived food.Samples were extracted with Na_2EDTA-Mcllvaine buffers,and purified by HLB and phosphoric acid solid phase extraction cartridge.Quantification of the analyte was achieved by HPLC with UV detector at 350 nm with acetonitrile-0.01mol/L TFA solvent mobile and using external standard calibration curves.Limits and quantification limits of this method for the analyte were 50μg/kg and 100μg/kg in liver,kindey,fat and skin of pig,cattle,sheep and chicken.The overall recovery varies from 61.0%~118.5%at the spiked level of 100μg/kg-1200μg/kg,the inter-batch coefficients was from 0.4%~14.5%.The method was sensitive and reproducibility,its performance can meet the requirements of the domestic and international legislation.The method adapts to the determination of Tetracylines residues in liver,kindey,fat and skin products.
A method based on high performance liquid chromatography(HPLC) has been developed for the determination of Tetracylines residues in animal derived food.Samples were extracted with Na_2EDTA-Mcllvaine buffers,and purified by HLB and phosphoric acid solid phase extraction cartridge.Quantification of the analyte was achieved by HPLC with UV detector at 350 nm with acetonitrile-0.01mol/L TFA solvent mobile and using external standard calibration curves.Limits and quantification limits of this method for the analyte were 50μg/kg and 100μg/kg in liver,kindey,fat and skin of pig,cattle,sheep and chicken.The overall recovery varies from 61.0%~118.5%at the spiked level of 100μg/kg-1200μg/kg,the inter-batch coefficients was from 0.4%~14.5%.The method was sensitive and reproducibility,its performance can meet the requirements of the domestic and international legislation.The method adapts to the determination of Tetracylines residues in liver,kindey,fat and skin products.
引文
[1]李俊锁,邱月明,王超.兽药残留分析[M].上海:上海科学技术出版社,2002:365-390.
[2]中华人民共和国农业部公告第235号《动物性食品中兽药最高残留限量》,2002:12-14
[3]岳正峰,郑卫平,谢丽琪等.高效液相色谱法测定动物组织中四环素类抗生素残留量的研究[J].分析实验室,2006,25(10):24-28
[4]庞国芳,曹彦忠,张进杰等.高效液相色谱法同时测定禽肉中土霉素、四环素、金霉素、强力霉素的研究[J].2005,24(4):61-63
[5]GB/T 20764-2006《可食性动物组织中土霉素、四环素、金霉素、强力霉素残留量的测定液相色谱-紫外检测法》
[6]GB/T 21317-2007《动物源性食品中四环素类兽药残留量的测定液相色谱-质谱,质谱法与高效液相色谱法》
[7]Posyniak A,Mitrowska K,Zmudzki J,et al.Analytical procedure for the determination of chlortetracycline and 4-ep-i chlortetracycline in pig kidneys[J].JChromatogrA,2005,1088(1-2):169-174.
[8]Dionex Application Note 329;Determination of Fat in Powdered Infant Formula Using Accelerated Solvent Extraction(ASE)
[2]中华人民共和国农业部公告第235号《动物性食品中兽药最高残留限量》,2002:12-14
[3]岳正峰,郑卫平,谢丽琪等.高效液相色谱法测定动物组织中四环素类抗生素残留量的研究[J].分析实验室,2006,25(10):24-28
[4]庞国芳,曹彦忠,张进杰等.高效液相色谱法同时测定禽肉中土霉素、四环素、金霉素、强力霉素的研究[J].2005,24(4):61-63
[5]GB/T 20764-2006《可食性动物组织中土霉素、四环素、金霉素、强力霉素残留量的测定液相色谱-紫外检测法》
[6]GB/T 21317-2007《动物源性食品中四环素类兽药残留量的测定液相色谱-质谱,质谱法与高效液相色谱法》
[7]Posyniak A,Mitrowska K,Zmudzki J,et al.Analytical procedure for the determination of chlortetracycline and 4-ep-i chlortetracycline in pig kidneys[J].JChromatogrA,2005,1088(1-2):169-174.
[8]Dionex Application Note 329;Determination of Fat in Powdered Infant Formula Using Accelerated Solvent Extraction(ASE)