液相色谱-四极杆-静电场轨道阱质谱结合改进的QuEChERS方法快速测定鸡蛋中多种抗病毒药物残留
详细信息 查看官网全文
- 英文论文题名：Rapid determination of antiviral drugs residues in eggs by LC-quadrupole-Orbitrap MS via modified QuEChERS method
- 论文作者：曲斌 ; 耿士伟 ; 陆桂萍 ; 蒋天梅 ; 刘善菁 ; 邵德佳 ; 陈蓉 ; 丁佳婧 ; 王芳 ; 温海燕
- 英文论文作者：QU Bin ; GENG Shi-wei ; LU Gui-ping ; JIANG Tian-mei ; LIU Shan-jing ; SHAO De-jia ; CHEN Rong ; DING Jia-jing ; WANG Fang ; WEN Hai-yan ; Jiangsu Quality Inspection and Testing Center for Animal Products ; China Pharmaceutical University ; ThermoFisher Technologies(China) Co.Ltd
- 年：2016
- 作者机构：江苏省畜产品质量检验测试中心;中国药科大学;赛默飞世尔科技(中国)有限公司;
- 论文关键词：鸡蛋 ; 抗病毒药物 ; QuEChERS ; LC-HRMS ; 残留
- 英文论文关键词：eggs ; antiviral drugs ; QuEChERS ; LC-HRMS ; veterinary drug residues
- 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：O657.63;S859.84
- 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：16
- 文件大小：2480k
- 原文格式：O
- 会议级别：全国
摘要
目的建立鸡蛋中利巴韦林、吗啉胍、金刚烷胺、金刚乙胺、阿昔洛韦、更昔洛韦等抗病毒药物残留的检测方法。方法使用改进的QuEChERS方法,鸡蛋样品经乙腈提取、EMR-lipid和C_(18)除脂,浓缩后经液相色谱-四极杆-静电场轨道阱质谱检测,采用Thermo Hypersil GOLD aO色谱柱(2.1×100 mm,1.9μm)分离,以0.1%甲酸和乙腈为流动相,梯度洗脱,内标法定量分析。结果上述六种目标化合物在7分钟内实现分离,峰形良好,在0.2~50μg/kg范围内线性良好(r~2>0.95)。鸡蛋中金刚烷胺和吗啉胍的检测限为0.1μg/kg,定量限为0.2μg/kg;利巴韦林、金刚乙胺、阿昔洛韦、更昔洛韦的检测限为0.2μg/kg,定量限为0.5μg/kg。高中低浓度日内、日间精密度小于15%,回收率在70%和120%之间。结论本方法经方法学验证,并将此方法应用于实际鸡蛋中抗病毒药物的检测,证明本方法灵敏度高,便捷、高效、实用。
Objective To develop a method for simultaneous determination of six antivirals,which include ribavirin,moroxydine,amantadine,rimantadine,acyclovir,ganciclovir,in eggs by modified QuEChERS method with LC-quadrupole-Orbitrap MS.Methods Antivirals in matrix,which was extracted by acetonitrile,purified with modified QuEChERS method.The sample were loaded onto Thermo Hypersil GOLD aQ column(2.1×100mm,1.9 μm) using gradient elution with aqueous solution(containing0.1%formic acid) /acetonitrile as mobile phase and tested by liquid chromatography-quadrupole-Orbitrap mass spectrometry.Stable isotopes were used as internal standard.Results Six antivirals were detected at the range of 0.5-50 μg/kg with good linearity which correlation coefficients(r~2) higher than 0.95.The limit of detection was 0.1 μg/kg for amantadine and moroxydine and 0.2 μg/kg for other 4 antivirals.The limit of quantification was 0.2 μg/kg for amantadine and moroxydine and 0.5 μg/kg for other 4 antivirals.The intra- and inter-precision were lower than 15%for high,medium and lower concentrations.The recoveries were between 70%and120%.Conclusion The method was proved capable for simultaneous determination of 6 antiviral residues in eggs after the method was applied to analysis 5 positive samples.It was shown that the method was simple,effective and accuracy as well.
Objective To develop a method for simultaneous determination of six antivirals,which include ribavirin,moroxydine,amantadine,rimantadine,acyclovir,ganciclovir,in eggs by modified QuEChERS method with LC-quadrupole-Orbitrap MS.Methods Antivirals in matrix,which was extracted by acetonitrile,purified with modified QuEChERS method.The sample were loaded onto Thermo Hypersil GOLD aQ column(2.1×100mm,1.9 μm) using gradient elution with aqueous solution(containing0.1%formic acid) /acetonitrile as mobile phase and tested by liquid chromatography-quadrupole-Orbitrap mass spectrometry.Stable isotopes were used as internal standard.Results Six antivirals were detected at the range of 0.5-50 μg/kg with good linearity which correlation coefficients(r~2) higher than 0.95.The limit of detection was 0.1 μg/kg for amantadine and moroxydine and 0.2 μg/kg for other 4 antivirals.The limit of quantification was 0.2 μg/kg for amantadine and moroxydine and 0.5 μg/kg for other 4 antivirals.The intra- and inter-precision were lower than 15%for high,medium and lower concentrations.The recoveries were between 70%and120%.Conclusion The method was proved capable for simultaneous determination of 6 antiviral residues in eggs after the method was applied to analysis 5 positive samples.It was shown that the method was simple,effective and accuracy as well.
引文
[1]FDA.FDAProhibits Use of Antiviral Drugs in Poultry to Help Keep Drugs Effective for Humans.[EB/OL].(2009-06-18)[2013-03-18].http://www.fda.gov/newsevents/newsroom/pressannouncements/2006/ucml08620.htm
[2]Wu XP,Wang WJ,Liu Y,et al.Development of an ELISA kit for the determination of amantadine in chicken muscle[J].J Inspection Quarantine,2015,24(4):68-70.
[3]Chan D,Tarbin J,Sharman M,et al.Screening method for the analysis of antiviral drugs in poultry tissues using zwitterionic hydrophilic interaction liquid chromatography/tandem mass spectrometry[J].Anal Chim Acta,2011,700:194-200.
[4]Liu ZC,Yang F,Yu KJ,et al.Multi-residue determination of five antiviral drugs in chicken tissues by liquid chromatography-electrospray ionization tandem mass spectrometry[J].Chin J Chromatogr,2012,30(12):1253-1259
[5]Turnipseed SB,Storey JM,Adersen WC,et al.Determination and confirmation of the antiviral drug amantadine and its analogues in chicken jerky pet treats[J].J Agric Food Chem,2015,63:6968-6978
[6]Berendsen BJA,Wegh RS,Essers ML,et al.Quantitative trace analysis of a broad range of antiviral drugs in poultry muscle using column-switch liquid chromatography coupled to tandem mass spectrometry[J].Anal Bioanal Chem,2012,402(4):1611-1623.
[7]Anastassiades M,Lehotay S J,Stajnbaher D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce[J].J AOAC Int,2003,86(2):412
[8]Wu YL,Chen RX,Xue Y,et al.Simultaneous determination of amantadine,rimantadine and memantine in chicken muscle using multi-walled carbon nanotubes as a reversed-dispersive solid phase extraction sorbent[J].J Chromatogr B,2014,965:197-205.
[9]Wu YL,Chen RX,Zhu L,et al.Determination of ribavirin in chicken muscle by quick,easy,cheap,effective,rugged and safe method and liquid chromatography-tandem mass spectrometry[J].J Chromatogr B,2016,1012-1013:55-60.
[2]Wu XP,Wang WJ,Liu Y,et al.Development of an ELISA kit for the determination of amantadine in chicken muscle[J].J Inspection Quarantine,2015,24(4):68-70.
[3]Chan D,Tarbin J,Sharman M,et al.Screening method for the analysis of antiviral drugs in poultry tissues using zwitterionic hydrophilic interaction liquid chromatography/tandem mass spectrometry[J].Anal Chim Acta,2011,700:194-200.
[4]Liu ZC,Yang F,Yu KJ,et al.Multi-residue determination of five antiviral drugs in chicken tissues by liquid chromatography-electrospray ionization tandem mass spectrometry[J].Chin J Chromatogr,2012,30(12):1253-1259
[5]Turnipseed SB,Storey JM,Adersen WC,et al.Determination and confirmation of the antiviral drug amantadine and its analogues in chicken jerky pet treats[J].J Agric Food Chem,2015,63:6968-6978
[6]Berendsen BJA,Wegh RS,Essers ML,et al.Quantitative trace analysis of a broad range of antiviral drugs in poultry muscle using column-switch liquid chromatography coupled to tandem mass spectrometry[J].Anal Bioanal Chem,2012,402(4):1611-1623.
[7]Anastassiades M,Lehotay S J,Stajnbaher D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce[J].J AOAC Int,2003,86(2):412
[8]Wu YL,Chen RX,Xue Y,et al.Simultaneous determination of amantadine,rimantadine and memantine in chicken muscle using multi-walled carbon nanotubes as a reversed-dispersive solid phase extraction sorbent[J].J Chromatogr B,2014,965:197-205.
[9]Wu YL,Chen RX,Zhu L,et al.Determination of ribavirin in chicken muscle by quick,easy,cheap,effective,rugged and safe method and liquid chromatography-tandem mass spectrometry[J].J Chromatogr B,2016,1012-1013:55-60.