牛奶中氨基糖苷类药物残留量的测定高效液相色谱串联质谱法
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- 英文论文题名：Determination of aminoglycosides in milk by high performance Liquid chromatography-tandem mass spectrometry
- 论文作者：方秋华 ; 刘佩怡 ; 肖田安 ; 吴荔琴 ; 伍宏凯 ; 梁祺琦 ; 何莹
- 英文论文作者：FANG Qiu-hua ; LIU Pei-yi ; XIAO Tian-an ; WU Li-qin ; WU Hong-kai ; LIANG Qi-qi ; HE Ying ; Guangdong Institute for Veterinary Drugs and Feedstuffs Control
- 年：2016
- 作者机构：广东省兽药饲料质量检验所;
- 论文关键词：氨基糖苷类 ; 牛奶 ; 残留 ; 高效液相色谱-串联质谱
- 英文论文关键词：aminoglycosides ; milk ; Residiues ; high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
- 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;O657.63
- 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：7
- 文件大小：750k
- 原文格式：O
- 会议级别：全国
摘要
本研究建立了高效液相色谱-串联质谱同时测定牛奶中链霉素、双氢链霉素、庆大霉素C1、卡那霉素、阿米卡星、大观霉素、安普霉素和新霉素等八种氨基糖苷类药物的多残留检测方法。试样用5%三氯乙酸提取,经Plexa固相萃取柱进一步净化,液相色谱分离,采用多反应监测正离子模式对八种氨基糖苷类药物同时进行定性定量分析。牛奶中八种氨基糖苷类药物的检测限为5μg/kg,定量限为10μg/kg。在牛奶中添加10,100,200,400μg/kg水平的药物回收试验中,平均回收率均在73.6%~117%之间,相对标准偏差为1.09%~9.60%。该方法灵敏、准确,适用于牛奶中氨基糖苷类药物残留的分析检测。
A confirmatory method has been developed and validated for the simultaneous determination of streptomycin(STREP),dihydrostreptomycin(DISTREP),gentamycin C1(GENT C1),kanamycin(KANA),amkacin(AMKI),spectinomycin(SPEC),apramycin(APRA) and neomycin(NEO) in milk using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The analytes were extracted from milk using 5%trichloroacetic acid(TCA),and then the sample extract were purified by Plexa solid-phase extraction.The analytes were analyzed by HPLC-MS/MS in positive multiple reaction monitoring(MRM) mode,acquiring two product ions from each of the chosen precursor ions for confirmation of the acetylgestagens.The limits of detection were 5 μg/kg for eight aminoglycosides,with quantification limits of 10 μg/kg.Recoveries were in the range 73.6%to 117%from milk fortified at the 100,200,400 μg/kg levels,and the mean intra-laboratory reproducibility ranged from 1.09%to 9.60%(%R.S.D).The developed method is sensitive and specific for the simultaneous detection of these aminoglycosides in milk.
A confirmatory method has been developed and validated for the simultaneous determination of streptomycin(STREP),dihydrostreptomycin(DISTREP),gentamycin C1(GENT C1),kanamycin(KANA),amkacin(AMKI),spectinomycin(SPEC),apramycin(APRA) and neomycin(NEO) in milk using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The analytes were extracted from milk using 5%trichloroacetic acid(TCA),and then the sample extract were purified by Plexa solid-phase extraction.The analytes were analyzed by HPLC-MS/MS in positive multiple reaction monitoring(MRM) mode,acquiring two product ions from each of the chosen precursor ions for confirmation of the acetylgestagens.The limits of detection were 5 μg/kg for eight aminoglycosides,with quantification limits of 10 μg/kg.Recoveries were in the range 73.6%to 117%from milk fortified at the 100,200,400 μg/kg levels,and the mean intra-laboratory reproducibility ranged from 1.09%to 9.60%(%R.S.D).The developed method is sensitive and specific for the simultaneous detection of these aminoglycosides in milk.
引文
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[2]Cazedey E C,Salgado H R.A novel and rapid microbiological assay for ciprofloxacin hydrochloride[J].Journal of Pharmaceutical Analysis,2013,3(5):382-386.
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[4]邓安平,杨秀岑,杨永明,等.用增强的化学发光免疫分析法测定血清中庆大霉素的含量[J].华西医科大学学报,1993.24(1):101-103.
[5]黄耀凌,刘智宏,叶妮,等.ELISA法检测牛奶中链霉素残留量[J].中国乳品工业,2007,35(2):54-56.
[6]钱疆,余孔捷,陈健,等.液相荧光法检测乳制品中9种氨基糖苷类药物残留[J]..福建分析测试,2011,20(3):13-17.
[7]Riichi Tawa,Hirokazu Matsunaga,Takashi Fujimoto,High-performance liquid chromatographic analysis of aminoglycoside antibiotics[J].Journal of Chromatography A,1998,812(1-2):141-150.
[8]孙雷,张骊,黄耀凌,等.超高效液相色谱-串联质谱法检测动物源食品中8种氨基糖苷类药物残留[J].质谱学报,2009.30(1):60-64.
[9]徐丽佳,刘笑,张秀芹,等.超高效液相色谱串联质谱法检测鸡蛋中残留的氨基糖苷类药物[J].药物分析杂志,2016,36(2):301-305.
[10]刘雪红,张秀芹,侯颖,等.超高效液相色谱-串联质谱法检测牛奶中7种氨基糖苷类药物残留[J].中国兽药杂志,2015,49(3):48-52.
[11]Commission decision(2002/657/EC).Official Journal of the European Communities,2002/L221/8~36.
[12]徐飞.氨基糖苷类药物残留检测筛选和确证方法的研究.博士学位论文,2014.
[13]李予雯,钟洪兰,刘思佳,等.高效液相色谱-串联质谱法检测3种氨基糖苷类抗结核药[J].现代医院,2016,16(6):851-853.
[14]苏晶,汤立忠,陈长毅,等.高效液相色谱串联质谱法同时测定9种龙虾中氨基糖苷类和四环素类抗生素残留[J].食品工业科技-分析检测,2016,37(2):60-67.
[15]高玲,张丹,高峰,等.水产品中氨基糖苷类药物残留的高效液相色谱-串联质谱检测方法研究[J].中国兽药杂志,2012,46(11):27-30.
[16]龚强,丁利,朱绍华,等.高效液相色谱-串联质谱法检测乳制品中10种氨基糖苷类抗生素残留[J].色谱,2012,30(11):1143-1147.
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[18]Wei xia Zhu,Ji zhou Yang,Wei Wei,et al.Simultaneous determination of 13 aminoglycoside residues in foods of animal origin by liquid chromatography-electrospray ionization tandem mass spectrometry with two consecutive solid-phase extraction steps[J].Journal of Chromatography A,2008,1207:29-37.
[19]安冬.水产品中氨基糖普类药物残留检测的液质联用分析法研究.硕士学位论文,2009.
[2]Cazedey E C,Salgado H R.A novel and rapid microbiological assay for ciprofloxacin hydrochloride[J].Journal of Pharmaceutical Analysis,2013,3(5):382-386.
[3]王苏华,周杨.鸡蛋中新霉素残留的微生物学检测方法[J].中国兽药杂志,2003,37(2):16-19.
[4]邓安平,杨秀岑,杨永明,等.用增强的化学发光免疫分析法测定血清中庆大霉素的含量[J].华西医科大学学报,1993.24(1):101-103.
[5]黄耀凌,刘智宏,叶妮,等.ELISA法检测牛奶中链霉素残留量[J].中国乳品工业,2007,35(2):54-56.
[6]钱疆,余孔捷,陈健,等.液相荧光法检测乳制品中9种氨基糖苷类药物残留[J]..福建分析测试,2011,20(3):13-17.
[7]Riichi Tawa,Hirokazu Matsunaga,Takashi Fujimoto,High-performance liquid chromatographic analysis of aminoglycoside antibiotics[J].Journal of Chromatography A,1998,812(1-2):141-150.
[8]孙雷,张骊,黄耀凌,等.超高效液相色谱-串联质谱法检测动物源食品中8种氨基糖苷类药物残留[J].质谱学报,2009.30(1):60-64.
[9]徐丽佳,刘笑,张秀芹,等.超高效液相色谱串联质谱法检测鸡蛋中残留的氨基糖苷类药物[J].药物分析杂志,2016,36(2):301-305.
[10]刘雪红,张秀芹,侯颖,等.超高效液相色谱-串联质谱法检测牛奶中7种氨基糖苷类药物残留[J].中国兽药杂志,2015,49(3):48-52.
[11]Commission decision(2002/657/EC).Official Journal of the European Communities,2002/L221/8~36.
[12]徐飞.氨基糖苷类药物残留检测筛选和确证方法的研究.博士学位论文,2014.
[13]李予雯,钟洪兰,刘思佳,等.高效液相色谱-串联质谱法检测3种氨基糖苷类抗结核药[J].现代医院,2016,16(6):851-853.
[14]苏晶,汤立忠,陈长毅,等.高效液相色谱串联质谱法同时测定9种龙虾中氨基糖苷类和四环素类抗生素残留[J].食品工业科技-分析检测,2016,37(2):60-67.
[15]高玲,张丹,高峰,等.水产品中氨基糖苷类药物残留的高效液相色谱-串联质谱检测方法研究[J].中国兽药杂志,2012,46(11):27-30.
[16]龚强,丁利,朱绍华,等.高效液相色谱-串联质谱法检测乳制品中10种氨基糖苷类抗生素残留[J].色谱,2012,30(11):1143-1147.
[17]Kwork D,Mori B,Yong M.Proceeding of the 45th ASMS Conference On MassSpectrometryand Applied Topics:American Society for Mass Spectrometry[J].Palm Springs CA:186-188.
[18]Wei xia Zhu,Ji zhou Yang,Wei Wei,et al.Simultaneous determination of 13 aminoglycoside residues in foods of animal origin by liquid chromatography-electrospray ionization tandem mass spectrometry with two consecutive solid-phase extraction steps[J].Journal of Chromatography A,2008,1207:29-37.
[19]安冬.水产品中氨基糖普类药物残留检测的液质联用分析法研究.硕士学位论文,2009.