HPLC-MS/MS法研究恩诺沙星在鸡蛋中残留消除规律

doi:10.12160/j.issn.1672-5190.2020.05.009

畜牧与饲料科学 ›› 2020, Vol. 41 ›› Issue (5): 46-51.doi: 10.12160/j.issn.1672-5190.2020.05.009

HPLC-MS/MS法研究恩诺沙星在鸡蛋中残留消除规律

侯轩, 周炜, 陈勇, 张航俊, 郭炫君, 张晓丽, 周芷锦

浙江省动物疫病预防控制中心, 浙江杭州 310020

收稿日期:2020-03-25 发布日期:2020-10-21
作者简介:侯轩（1988—）, 男, 兽医师, 硕士, 主要从事兽药和畜产品质量安全检测工作。

Investigation of Residues and Elimination Regularity of Enrofloxacin in Chicken Eggs by using HPLC-MS/MS

HOU Xuan, ZHOU Wei, CHEN Yong, ZHANG Hang-jun, GUO Xuan-jun, ZHANG Xiao-li, ZHOU Zhi-jin

Zhejiang Animal Disease Prevention and Control Center, Hangzhou 310020, China

Received:2020-03-25 Published:2020-10-21

摘要/Abstract

摘要： 建立了高效液相色谱—串联质谱法（HPLC-MS/MS）检测鸡蛋中恩诺沙星、环丙沙星残留的方法。鸡蛋样品经1%乙酸乙腈提取、正己烷除脂, 用HPLC-MS/MS进行检测。恩诺沙星、环丙沙星在0.5~500 ng/mL浓度时线性关系良好（r≥0.999）;恩诺沙星回收率为87.7%~99.1%、环丙沙星的回收率为89.1%~101.4%, 检测限为0.5 μg/kg, 定量限为1.0 μg/kg。应用该方法初步研究了恩诺沙星及其代谢物环丙沙星在鸡蛋中的残留消除规律。结果表明, 给药后鸡蛋中恩诺沙星及其代谢物蓄积迅速, 停药8 d后痕量恩诺沙星代谢缓慢, 25 d后恩诺沙星代谢完全。

关键词: 恩诺沙星, 环丙沙星, 鸡蛋, 高效液相色谱—串联质谱法;

Abstract: A method for determination of enrofloxacin and ciprofloxacin residues in chicken eggs was developed using high-performance liquid chromatography coupled with tandem mass spectrometry （HPLC-MS/MS）. After extraction by 1% acetic acid in acetonitrile and purified by hexane, the samples were analyzed by the established HPLC-MS/MS method. The calibration curves of enrofloxacin and ciprofloxacin were linear in the range of 0.5-500 ng/mL （r ≥ 0.999）; the recoveries of enrofloxacin in chicken eggs ranged from 87.7% to 99.1%, and those of ciprofloxacin in the samples ranged from 89.1% to 101.4%; the limit of detection and the limit of quantification of the established HPLC-MS/MS method for enrofloxacin and ciprofloxacin were 0.5 μg/kg and 1.0 μg/kg, respectively. The residues and elimination regularity of enrofloxacin and its metabolite ciprofloxacin in chicken eggs were preliminarily revealed by using a HPLC-MS/MS based method the enrofloxacin and its metabolite were accumulated rapidly in eggs after the chicken were administrated, the metabolism of trace enrofloxacin was slow after 8 days of drug discontinuation, and the metabolism of enrofloxacin was complete after 25 days of drug discontinuation.

Key words: enrofloxacin, ciprofloxacin, chicken eggs, HPLC-MS/MS

中图分类号:

侯轩, 周炜, 陈勇, 张航俊, 郭炫君, 张晓丽, 周芷锦. HPLC-MS/MS法研究恩诺沙星在鸡蛋中残留消除规律[J]. 畜牧与饲料科学, 2020, 41(5): 46-51.

HOU Xuan, ZHOU Wei, CHEN Yong, ZHANG Hang-jun, GUO Xuan-jun, ZHANG Xiao-li, ZHOU Zhi-jin. Investigation of Residues and Elimination Regularity of Enrofloxacin in Chicken Eggs by using HPLC-MS/MS[J]. Animal Husbandry and Feed Science, 2020, 41(5): 46-51.

参考文献

[1] KNOLL U, GLÜNDER G, KIETZMANN M. Comparative study of the plasma pharmacokinetics and tissue concentrations of danofloxacin and enrofloxacin in broiler chickens[J].Journal of Veterinary Pharmacology and Therapeutics, 1999, 22(4):239-246.
[2] 李俊锁, 邱月明, 王超.兽药残留分析[M].上海:上海科技出版社, 2002:365-390.
[3] HE X T, DENG M S, WANG Q, et al.Residues and health risk assessment of quinolones and sulfonamides in cultured fish from Pearl River Delta, China[J].Aquaculture, 2016, 458:38-46.
[4] OVANDO H G, GORLA N, LUDERS C, et al.Comparative pharmacokinetics of enrofloxacin and ciprofloxacin in chickens[J].Journal of Veterinary Pharmacology and Therapeutics, 1999, 22(3):209-212.
[5] 张萍. 鸡蛋中抗生素类药物残留的研究进展[J].北方药学, 2015, 12(4):90-92.
[6] 丁国华, 丁磊如, 刘霞.氟喹诺酮类药的神经毒性作用[J].中国医院药学杂志, 1995(8):380-381.
[7] 高晓月, 范维, 陈淑敏, 等.微生物显色法检测禽畜肉中混合抗生素残留[J].肉类研究, 2019, 33(4):36-41.
[8] 孙雷, 朱馨乐, 刘琪, 等.猪肉组织中7种氟喹诺酮类药物残留检测高效液相色谱—串联质谱法研究[J].中国兽药杂志, 2008(3):12-15.
[9] 高何刚, 王瑞, 杜赛, 等.超高效液相色谱—串联质谱联用法同时测定鸡肉中磺胺和喹诺酮类兽药残留[J].中国卫生检验杂志, 2017, 27(17):2481-2485.
[10] 董昕. UPLC-MS/MS法同时测定动物油脂中11种喹诺酮类兽药残留[J].上海计量测试, 2019, 46(4):22-25.
[11] 中华人民共和国农业农村部.动物性食品中氟喹诺酮类药物残留检测高效液相色谱法:农业农村部1025号公告-14-2008[S].北京:中国标准出版社, 2008.
[12] 孙思, 王安波, 杨梅, 等.超高效液相色谱法检测鸡蛋中4种氟喹诺酮类药物残留[J].贵州农业科学, 2018, 46(1):104-108.
[13] KIM Y, JUNG J, KIM M, et al.Prioritizing veterinary pharmaceuticals for aquatic environment in Korea[J].Environmental Toxicology and Pharmacology, 2008, 26(2):167-176.

[1]	董复成,李建慧,苏蕊,张雪,张可可,秦鑫,陈晨,王文玲,曹靖. 鸡蛋暗斑对蛋品质及抗氧化能力的影响[J]. 畜牧与饲料科学, 2018, 39(7): 19-19.
[2]	崔卫涛,代娟,吴贝,况世昌,刘爽,李雄,柯志中,李钢平,李筱雯. 联合使用发酵饲料和发酵中草药微生态制剂替代饲用抗生素对蛋鸡的影响与研究[J]. 畜牧与饲料科学, 2018, 39(11): 27-30.
[3]	薛艳蓉,茂文,赵瑞生,王呈,刘波,李建国. 鸡蛋在储存过程中微生物及蛋品质的变化研究[J]. 畜牧与饲料科学, 2017, 38(8): 67-67.
[4]	沙其拉,黎明. 凡士林涂抹法与冷藏法对鸡蛋保鲜效果影响的比较研究[J]. 畜牧与饲料科学, 2017, 38(5): 100-100.
[5]	王琳,王飞. 姜黄对蛋鸡生产性能、鸡蛋品质和血清生化指标的影响[J]. 畜牧与饲料科学, 2017, 38(2): 32-32.
[6]	徐静,陈巧尔,俞耀飞,沈淳,李银蝶. 不同品种鸡蛋蛋清溶菌酶粗提率及蛋清抑菌效果的比较[J]. 畜牧与饲料科学, 2017, 38(1): 16-16.
[7]	冯静,王燕,臧蕾,刘会杰,鹏达,马雪英. 不同品种蛋鸡鸡蛋营养成分的比较研究[J]. 畜牧与饲料科学, 2016, 37(9): 4-4.
[8]	冯静. 拉萨白鸡鸡蛋营养成分的分析[J]. 畜牧与饲料科学, 2016, 37(12): 23-23.
[9]	冯静. 3个品种鸡的蛋品质比较研究[J]. 畜牧与饲料科学, 2016, 37(11): 12-12.
[10]	冯静,马雪英,王燕,臧蕾,鹏达. 拉萨白鸡蛋品质的测定及相关分析[J]. 畜牧与饲料科学, 2016, 37(10): 10-10.
[11]	丛琳,武瑞,李银生. 恩诺沙星对细胞色素P450酶系影响的研究进展[J]. 畜牧与饲料科学, 2016, 37(1): 34-34.
[12]	朱奇平,唐韵,宣柯,韦力,丁国骅. 不同品种鸡蛋品质及蛋黄中热量和性激素含量的比较[J]. 畜牧与饲料科学, 2015, 36(5): 4-4.
[13]	徐有均. 鸡蛋的营养价值[J]. 畜牧与饲料科学, 2012, 33(9): 116-116.
[14]	黄芝生. 提高种鸡蛋孵化率的有效措施[J]. 畜牧与饲料科学, 2011, 32(4): 126-126.
[15]	邓鸿铃,苏新国. 鸡蛋中黄体酮等激素含量的检测分析研究[J]. 畜牧与饲料科学, 2011, 32(2): 55-55.

HPLC-MS/MS法研究恩诺沙星在鸡蛋中残留消除规律

Investigation of Residues and Elimination Regularity of Enrofloxacin in Chicken Eggs by using HPLC-MS/MS

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价