超高压液相色谱-静电场轨道阱高分辨质谱筛查渔用饲料中175种药物

来源 :分析试验室 | 被引量 : 0次 | 上传用户:aspbasicer
下载到本地 , 更方便阅读
声明 : 本文档内容版权归属内容提供方 , 如果您对本文有版权争议 , 可与客服联系进行内容授权或下架
论文部分内容阅读
建立了超高压液相色谱-静电场轨道阱高分辨质谱快速筛查渔用饲料中多种类药物残留的方法.饲料样品经1%甲酸乙腈溶液提取, 浓缩复溶后加水稀释, 离心除沉淀, 以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相, 经Accucore RP-MS色谱柱 (100 mm×2.1 mm i.d., 2.6μm) 梯度洗脱分离, H-ESI (Heated Electrospray Ionization) 离子化, 采用Full M S/dd-M S2 (Top N) 模式采集数据, 利用自建的数据库进行定性分析.当满足母离子质荷比偏差<3×10-6;保留时间偏差<15 s;同位素质荷比偏差<1×10-5、相对丰度偏差75%;碎片离子质荷比偏差<2×10-5且至少有一个碎片与数据库中匹配时认为确证检出.方法在200μg/kg可同时定性确证175种药物, 50μg/kg同时定性确证136种药物, 10μg/kg同时定性确证116种药物, RSD<30%, 母离子相对偏差均小于1.9×10-6.200μg/kg加标时, 81%的化合物回收率在30%~110%之间.“,”A rapid screening method of 175 veterinary drug residues in fishery feed based on simple and fast pretreatment and ultrahigh performance liquid chromatography coupled to quadrupole-orbitraphigh resolution mass spectrometer (UPLC-Q-Orbitrap HRMS)was established. In this method, analytes in samples were extracted with 1% (V/V)formic acid in acetonitrile, The extract was then with N2 and redissolved with 1% (V/V)formic acid in acetonitrile. Clean-up procedure was achieved by adding isometric water and centrifuged at 5℃, 10000 r/min for 10 minutes to discard precipitation.Then, 175 target compounds were separated on an Accucore RP-MS (100 mm × 2. 1 mm i. d., 2. 6 μm)column, with 0. 1% formic acid in water and 0. 1% formic acid in acetonitrile as mobile phase. An H-ESI ion source was employed and the data were acquired under Full MS/dd-MS2 (Top N)mode with an inclusion list covering 175 compounds. In the process of qualification, the allowed precursor ion m/z tolerance was set at 3 × 10-6, RT override window set as ± 15 seconds, allowed product ion m/z tolerance set as 2 × 10-5 because of the existence of some product ions with m/z less than 100 and at least 1 product ion was required for qualification, allowed isotope m/z deviation set as1 × 10-5, intensity deviation as 25% and fit threshold as 75%. In our work, 175 compounds belonging to 18 categories were eluted within 20 minutes, and were identified with this method at200 μg/kg. Also, 136 and 116 compounds were identified at 50 μg/kg and 10 μg/kg, respectively.
其他文献
《义务教育数学课程标准》中要求:学会独立思考,体会数学的基本思想和思维方式。初步学会从数学的角度发现问题和提出问题,综合运用数学知识解决简单的实际问题,增强应用意识
期刊
采用分散固相萃取净化,亲水作用色谱串联质谱分离检测,建立了荸荠中高氯酸盐的检测方法.对荸荠中高氯酸盐的提取和净化条件进行了优化:提取溶剂为含1%乙酸的乙腈/水(V∶V,1∶1