超高压液相色谱串联高分辨质谱筛查渔用投入品中禁限用药物

发布时间：2018-10-26 09:38

【摘要】：建立了超高压液相色谱-静电场轨道离子阱质谱系统对渔用投入品中可能造成风险隐患的禁限用药物的快速筛查与定量技术。以水(含1%甲酸)-乙腈(1∶9,V/V)溶液进行提取,通过稀释降低基质效应,在Accucore RP-MS色谱柱(100 mm×2.1 mm,2.6μm)上,以水(含0.1%甲酸)和乙腈(含0.1%甲酸)溶液为流动相,利用梯度洗脱、HESI离子化,Full-scan dd MS2(Top N)扫描模式进行数据采集,通过与预先建立好的药物标准品质谱、色谱数据库进行比对分析,实现了53种禁限用药同时筛查确证与定量分析。各药物最低检出浓度均低于10 ng/mL,在0.01~1.0μg/mL范围内,各药物的线性相关系数均大于0.98,根据实际测定结果设定对渔药及渔用饲料中筛查药物的检出限分别为0.5和5.0 mg/L,对渔药及渔用饲料基质添加10和100 mg/kg的各筛查成分,定量回收率均高于50%,相对标准偏差均小于15%。将本方法用于农业部渔用投入品质量安全隐患排查项目中,共筛查68个样品,其中在29个渔用兽药样品中筛查出15种说明书中未标明成分。
[Abstract]:A rapid screening and quantification technique for prohibitive drugs in fishery inputs, which may cause potential risks, was established by ultra-high pressure liquid chromatography-electrostatic field orbital ion trap mass spectrometry system. Water (containing 1% formic acid) -acetonitrile (1: 9 V / V) solution was extracted, and the matrix effect was reduced by dilution. The extraction was carried out on a Accucore RP-MS column (100 mm 脳 2.1 mm,2.6 渭 m). Using water (0.1% formic acid) and acetonitrile (0.1% formic acid) as mobile phase, gradient elution, HESI ionization and Full-scan dd MS2 (Top N) scanning mode were used for data acquisition. By comparing and analyzing with the pre-established drug standard mass spectrometry and chromatographic database, 53 kinds of proscribed drugs were screened and confirmed and quantitatively analyzed at the same time. The lowest detectable concentration of each drug was less than 10 ng/mL, and the linear correlation coefficient of each drug was more than 0.98 in the range of 0.01 渭 g/mL. According to the actual results, the detection limits of fish drugs and fish feed screening drugs were set to be 0.5 mg/L, and 5.0 mg/L, respectively, and the quantitative recovery rates were all higher than 50%, when 10 and 100 mg/kg were added to the fish medicine and fishery feed substrate, respectively. The relative standard deviations are less than 15. The method has been applied to the hidden trouble investigation of fishery inputs in the Ministry of Agriculture, and 68 samples were screened, of which 15 were not marked in the specification of 29 veterinary drug samples.
【作者单位】：东海水产研究所水产品质量安全与加工实验室;赛默飞世尔科技(中国)有限公司;
【基金】：上海市农业科学委员会(沪农科推字(2016)第1-4-1号) 中央级公益性科研院所基本科研业务费专项资金(中国水产科学研究院东海水产研究所)(No.2014T05) 上海市科学技术委员会扬帆人才计划项目(No.14YF1408100)资助
【分类号】：S948;O657.63

【相似文献】