鸡组织中硫酸头孢喹肟的残留检测——高效液相色谱法
[目的]为了检测鸡组织中硫酸头孢喹肟的残留,建立了测定鸡组织中硫酸头孢喹肟残留的高效液相色谱法(HPLC)。[方法]取皮脂、肌肉、肝脏、肾脏4种组织匀浆,按照体积比20∶1的比例分别添加硫酸头孢喹肟标准品,制成的生物样品经乙腈-水(体积比为1∶11)提取,正己烷去脂,固相萃取柱富集净化,收集洗脱液在50℃水浴条件下N2吹干后复溶,在C18色谱柱上进行分离,紫外检测器(270 nm)下检测。以甲酸调节的p H3.0左右的乙腈-水溶液(体积比为1∶10)作为流动相。[结果]该方法测得硫酸头孢喹肟在皮脂、肌肉、肝脏、肾脏等组织中的检测限均为0.01μg·g-1,定量限均为0.02μg·g-1;各个组...
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Published in | 南京农业大学学报 Vol. 40; no. 5; pp. 894 - 900 |
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Main Author | |
Format | Journal Article |
Language | Chinese |
Published |
瑞普(天津)生物药业有限公司,天津300308
2017
南京农业大学动物医学院,江苏南京,210095%瑞普(天津)生物药业有限公司,天津,300308%南京农业大学动物医学院,江苏南京210095 |
Subjects | |
Online Access | Get full text |
ISSN | 1000-2030 |
DOI | 10.7685/jnau.201701018 |
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Summary: | [目的]为了检测鸡组织中硫酸头孢喹肟的残留,建立了测定鸡组织中硫酸头孢喹肟残留的高效液相色谱法(HPLC)。[方法]取皮脂、肌肉、肝脏、肾脏4种组织匀浆,按照体积比20∶1的比例分别添加硫酸头孢喹肟标准品,制成的生物样品经乙腈-水(体积比为1∶11)提取,正己烷去脂,固相萃取柱富集净化,收集洗脱液在50℃水浴条件下N2吹干后复溶,在C18色谱柱上进行分离,紫外检测器(270 nm)下检测。以甲酸调节的p H3.0左右的乙腈-水溶液(体积比为1∶10)作为流动相。[结果]该方法测得硫酸头孢喹肟在皮脂、肌肉、肝脏、肾脏等组织中的检测限均为0.01μg·g-1,定量限均为0.02μg·g-1;各个组织在0.02~2.00μg·g-1范围内线性关系良好,相关系数(R2)均大于0.99;添加高、中、低(2.00、0.20、0.02μg·g-1)含量的硫酸头孢喹肟后,其在皮脂、肌肉、肝脏、肾脏中的平均回收率分别为89.46%、88.85%、89.90%、85.98%;日内变异系数0.86%~11.8%,日间变异系数2.44%~11.13%,均符合添加回收率和变异系数的规定;含有药物的生物样品在常温、4℃及-20℃保存48 h条件下均不降解,稳定性好;在匀浆组织中添加与硫酸头孢喹肟结构及性质相近的4种药物(阿莫西林、甲氧苄啶、氨苄西林、磺胺嘧啶),均不会干扰硫酸头孢喹肟的检测。[结论]建立的检测鸡组织中硫酸头孢喹肟残留的HPLC法精确度高,准确性和重现性好,符合残留检测的要求。 |
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Bibliography: | 32-1148/S LI Qiaoning1 , ZHAO Jie1 , LIU Ailing2, MENG Xiaobin2, BAO Endong1,2 ( 1. College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, China ; 2.Ringpu(Tianjin) Bio-pharmacy Co. Ltd. ,Tianjin 300308, China) [ Objectives ] In order to detect the residues of cefquinome sulfate in broiler tissues, the solid-phase extraction and high performance liquid chromatography(HPLC) for determination of cefquinome sulfate residues in broiler tissues was established in this paper. [ Methods] Cefquinome sulfate was added to the homogenized samples such as skin+fat ,muscle ,liver and kidney according to the volume proportion at 20 : 1. After being mixed with samples totally, the cefquinome sulfate was extracted from biological samples by water and acetonitrile( measuring 99 mL purified water, add 9 mL of acetonitrile, mixing it up). The supernatant was oscillated for 15 rain with 6 mL of N-bexane to degrease fat and then cleaned up on SPE column. The eluent was collected and dried under nitrogen ev |
ISSN: | 1000-2030 |
DOI: | 10.7685/jnau.201701018 |