超高效液相色谱-四级杆-静电场轨道肼高分辨质谱筛查测定饲料中19种磺胺类药物
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- 英文论文题名：Screening and confirmation of 19 sulfonamides in feed by ultra high performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry
- 论文作者：严凤 ; 李丹妮 ; 吴剑平 ; 周哲 ; 张鑫 ; 潘娟 ; 张婧
- 英文论文作者：YAN Feng ; LI Dan-ni ; Wu Jian-pin ; Zhou Zhe ; Zhang Xin ; Pan Juan ; Zhang Jing ; Shanghai Municipal Supervisory Institute Veterinary Drugs and Feedstaff ; Thermofisher scientific(china)
- 年：2016
- 作者机构：上海市兽药饲料检测所;赛默飞世尔科技(中国);
- 论文关键词：超高效液相色谱 ; 四级杆-静电场轨道阱高分辨质谱 ; 磺胺类 ; 饲料
- 英文论文关键词：ultra high performance liquid chromatography(UPLC) ; quadrupole-exactive orbitrap ; sulfonamides ; feed
- 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：S816.17
- 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：9
- 文件大小：1228k
- 原文格式：O
- 会议级别：全国
摘要
建立了超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用(UPLC-Q-Exactive Orbitrap)快速筛查和确证定量饲料中19种磺胺类药物的分析方法。饲料样品经乙腈-0.1%甲酸溶液(80:20,v/v)超声提取,用Agilent SB C_(18)色谱柱(100mm×3.0mm,1.8μm)分离,以0.1%(v/v)甲酸乙腈溶液和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱。通过静电场轨道阱全扫描得到磺胺类药物的一级精确质量数与理论精确相对分子质量对比,相对质量偏差在0.006×10~(-6)~1.252×10~(-6)之间,有效地去除了基质干扰,实现对饲料中磺胺类药物的快速筛查;建立了19种磺胺类药物的二级质谱数据库,实现对19种磺胺类药物的定性筛查及同步定量。19种磺胺类药物在0.1~200μg/L浓度范围内线性关系良好r>0.99,方法检测限为50μg/kg,回收率为59.61%~106.45%。
An ultra high performance liquid chromatography- quadrupole-exactive orbitrap mass spectrometry method(UPLC-Q-Exactive Orbitrap) was developed for rapid screening,confirmation and quantitative of 19 sulfonamides in feed.The samples were extracted with acetonitrile-0.1%aqueous formic acid solution(80:20,v/v),and the extracts were then separated on an Agilent SB C_(18)(50 mm×3.0mm,1.8 μm) using a binary solvent system composed of 0.1%formic acid acetonitrile solution and 0.1%aqueous formic acid solution by gradient elution.The relative molecular masses of the target compounds were obtained in full scan mode with a relative deviation in the range of 0.006×10~(-6)~1.252×10~(-6) compared to the theoretical value,indicating effective elimination of the matrix interference.Tandem mass spectrometric database based on characteristic fragment ions for the 19 sulfonamides was built.This method allowed qualitative screening and quantitative analysis at the same time.Calibration curve was linear between 0.1 and 200μg/L,with the correlation coefficient r>0.99.The limit of detection was 50μg/kg.The recovery in feed was59.61%~106.45%.
An ultra high performance liquid chromatography- quadrupole-exactive orbitrap mass spectrometry method(UPLC-Q-Exactive Orbitrap) was developed for rapid screening,confirmation and quantitative of 19 sulfonamides in feed.The samples were extracted with acetonitrile-0.1%aqueous formic acid solution(80:20,v/v),and the extracts were then separated on an Agilent SB C_(18)(50 mm×3.0mm,1.8 μm) using a binary solvent system composed of 0.1%formic acid acetonitrile solution and 0.1%aqueous formic acid solution by gradient elution.The relative molecular masses of the target compounds were obtained in full scan mode with a relative deviation in the range of 0.006×10~(-6)~1.252×10~(-6) compared to the theoretical value,indicating effective elimination of the matrix interference.Tandem mass spectrometric database based on characteristic fragment ions for the 19 sulfonamides was built.This method allowed qualitative screening and quantitative analysis at the same time.Calibration curve was linear between 0.1 and 200μg/L,with the correlation coefficient r>0.99.The limit of detection was 50μg/kg.The recovery in feed was59.61%~106.45%.
引文
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[10]吴宁鹏.班付国.彭丽等.超高效液相色谱-串联四极杆飞行时间质谱法筛查饲料中11种镇静剂类药物[J].质谱学报2012,33(2):94-98.117.
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[2]赵书景.贺绍君.罗国琦等.动物性食品中磺胺类药物残留检测方法的研究进展[J].中国畜牧兽医,2009,36(8):60-63.
[3]GB/T 19542-2007饲料中磺胺类药物的测定—高效液相色谱法[S].北京:中国标准出版社,2007.
[4]陈吉之.闫超.饲料中9种磺胺类药物的HPLC法快速分离与检测中国医药工业杂志[J].2015,46(8):892-894.
[5]陈文慧.高效液相色谱-串联质谱法测定饲料中九种磺胺类药物的残留量[J].分析试验室,2010,29(9):52-56.
[6]罗辉泰.黄晓兰.吴惠勤等.分散固相萃取/高效液相色谱-串联质谱法快速测定饲料中87种药物残留[J].分析测试学报2015,34.(9):979-985.
[7]熊岑.李苑雯.郑彦婕等.静电场轨道阱质谱分析技术在食品分析中的应用进展[J].食品科学,2015,36(13):283-287.
[8]姚凤花.冯永巍.高效液相色谱串联飞行时间质谱法快速检测饲料中多种β-受体激动剂[J]粮食与饲料工业,2013,1:62-64.
[9]贡松松.顾欣.曹慧等.超高效液相色谱-四极杆飞行时间质谱法快速筛查生鲜牛乳中的14种磺胺类药物[J].分析测试学报2014,33(12):1342-1348.
[10]吴宁鹏.班付国.彭丽等.超高效液相色谱-串联四极杆飞行时间质谱法筛查饲料中11种镇静剂类药物[J].质谱学报2012,33(2):94-98.117.
[11]李明.马家辰.李红梅等.静电场轨道阱质谱的进展[J].质谱学报2013,34(3):185-192.