[1]张伟,彭麟,江善祥.超高效液相色谱-串联质谱法测定畜禽饲料中氯霉素类药物含量[J].南京农业大学学报,2015,38(3):453-458.[doi:10.7685/j.issn.1000-2030.2015.03.015]
 ZHANG Wei,PENG Lin,JIANG Shanxiang.Determination of chloramphenicols in the livestock and poultry feeds by UPLC-MS/MS[J].Journal of Nanjing Agricultural University,2015,38(3):453-458.[doi:10.7685/j.issn.1000-2030.2015.03.015]
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超高效液相色谱-串联质谱法测定畜禽饲料中氯霉素类药物含量()
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《南京农业大学学报》[ISSN:1000-2030/CN:32-1148/S]

卷:
38卷
期数:
2015年3期
页码:
453-458
栏目:
出版日期:
2015-05-14

文章信息/Info

Title:
Determination of chloramphenicols in the livestock and poultry feeds by UPLC-MS/MS
作者:
张伟 彭麟 江善祥
南京农业大学动物医学院, 江苏 南京 210095
Author(s):
ZHANG Wei PENG Lin JIANG Shanxiang
College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, China
关键词:
超高效液相色谱-串联质谱氯霉素甲砜霉素氟苯尼考畜禽饲料
Keywords:
UPLC-MS/MSchloramphenicolthiamphenicolflorfenicollivestock and poultry feeds
分类号:
S859.79
DOI:
10.7685/j.issn.1000-2030.2015.03.015
摘要:
[目的] 建立一种畜禽饲料中氯霉素、甲砜霉素和氟苯尼考的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,为监控畜禽饲料中违法添加该类药物提供方法指导,保障动物源食品安全。[方法] 饲料粉碎后,经碱性乙酸乙酯提取,正己烷除脂,Sep-Pak C18固相萃取柱净化,Waters Acquity UPLC BEH C18色谱柱分离,采用乙腈和水为流动相,并用梯度洗脱来提高对3种药物的分离能力。分别以d5-氯霉素、d3-甲砜霉素和d3-氟苯尼考为内标,采用负离子多反应监测模式,6个特征离子通道(m/z:321→152,257;354→185,290;356→185,336)用于氯霉素、甲砜霉素和氟苯尼考的定性和定量检测。[结果] 3种氯霉素类药物在1~20 μg·kg-1范围内线性良好,相关系数均大于0.99,方法检测限为0.1 μg·kg-1,定量限为0.3 μg·kg-1。3个加标水平(1、2和5 μg·kg-1)的平均回收率为81.41%~112.88%,日内精密度为1.24%~12.92%,日间精密度为0.64%~13.09%。[结论] 试验结果完全符合氯霉素类药物检测的相关法规要求,适用于畜禽饲料中氯霉素类药物的定性定量检测。
Abstract:
[Objectives] The aim of this experiment was to establish a detection method for chloramphenicol, thiamphenicol, and florfenicol by ultra performance liquid chromatography-tandem mass spectrometry in the livestock and poultry feeds, which could provide a methodological guidance to monitor these medicinal additives which were illegally added in the feed and further ensure the safety of animal origin food. [Methods] The ground samples were extracted with a mixture of ammonia water/ethyl acetate by liquid-liquid extraction, and the fat was removed by hexane. Sep-Pak C18solid phase extraction columns were used to clean up the impurities from the matrix. The separation step of chloramphenicol, thiamphenicol, and florfenicol was performed on Waters Acquity UPLC system with a column of BEH C18. The mobile phase was acetonitrile and water, and the gradient elution program was used to improve the separating capacity. d5-chloramphenicol, d3-thiamphenicol and d3-florfenicol were used as the mixed internal standards and drug monitoring mode was negative ion multiple reaction monitoring mode. Six characteristic transition reactions(m/z:321→152, 257;354 →185, 290;356→185, 336)were tested for the confirmation and quantification of chloramphenicol, thiamphenicol and florfenicol simultaneously. [Results] The results showed that the calibration curves were good linear at the concentrations of 1-20 μg·kg-1. The relative coefficients(R2)were greater than 0.99. The limit of detection of chloramphenicol, thiamphenicol and florfenicol was 0.1 μg·kg-1 and the limit of quantification was 0.3 μg·kg-1. The average recoveries of 3 drugs at the concentrations of 1, 2, 5 μg·kg-1 ranged from 81.41% to 112.88%. The intra-day RSD of this method was 1.24%-12.92%, inter-day RSD was 0.64%-13.09%. [Conclusions] The test results were fully in line with the related regulatory requirements and the method could be used to detect chloramphenicol, thiamphenicol, florfenicol in the livestock and poultry feeds.

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相似文献/References:

[1]黄世乐,陈祖义,成冰.畜产品中氯霉素的放射免疫测定[J].南京农业大学学报,1991,14(03):109.[doi:10.7685/j.issn.1000-2030.1991.03.022]
 Huang Shile,Chen Zuyi,Cheng Bing.RADIOIMMUNOASSAY FOR CHLORAMPHENICOL IN ANIMAL PRODUCTS[J].Journal of Nanjing Agricultural University,1991,14(3):109.[doi:10.7685/j.issn.1000-2030.1991.03.022]

备注/Memo

备注/Memo:
收稿日期:2014-11-25。
基金项目:农业部农业行业标准修订项目(2013-086)
作者简介:张伟,硕士研究生。
通讯作者:江善祥,教授,博导,研究方向为兽医药理及新兽药研制,E-mail:nauvy@sina.com。
更新日期/Last Update: 1900-01-01