高效液相色谱-串联质谱法测定养殖环境沉积物中多肽类抗生素残留量

发布时间：2018-12-09 18:38

【摘要】：建立了测定水产养殖环境沉积物中多肽类抗生素残留量的高效液相色谱串联质谱法。沉积物经10 m L甲醇-柠檬酸-Na_2HPO_4溶液(3∶4,V/V)超声提取2次,0.5 g乙二胺四乙酸二钠络合除杂,5 m L甲基异丁基甲酮净化,HLB固相萃取柱进一步富集净化,MGII C18色谱柱分离,0.1%甲酸与0.1%甲酸-乙腈梯度洗脱,ESI+电离,多反应监测模式(MRM)监测,外标法定量。粘菌素和杆菌肽在10~10000μg/L范围内,维吉尼霉素M1在4~4000μg/L范围内,线性回归系数均大于0.999,方法检出限为2~5μg/kg,方法定量限为4~10μg/kg。在3个浓度添加水平下,多肽类抗生素回收率79.7%~91.6%,相对标准偏差1.9%~10.8%。本方法具有良好的精密度和准确度,灵敏度高,适用范围广。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC / MS) method was developed for the determination of polypeptide antibiotic residues in aquaculture sediments. The sediment was extracted twice with 10 mL methanol-citric acid Na_2HPO_4 solution (3: 4 V / V), 0.5 g ethylenediamine tetraacetic acid disodium complex to remove impurities, and 5 mL methyl isobutyl ketone was purified. HLB solid phase extraction column was further enriched and purified, MGII C18 column was separated, 0.1% formic acid and 0.1% formic acid-acetonitrile were eluted gradient, ESI ionization, multi-reaction monitoring model (MRM) monitoring, external standard method quantitative analysis. The linear regression coefficients of myxin and bacitracin in the range of 1010 000 渭 g / L, vigniomycin M1 4 000 渭 g / L, the detection limit of 2 ~ 5 渭 g / kg and the quantitative limit of 4 ~ 10 渭 g / kg were all greater than 0.999. The recovery rate of polypeptide antibiotics was 79.7% and 91.6%, and the relative standard deviation was 1.9%, 10.8%. The method has good precision and accuracy, high sensitivity and wide range of application.
【作者单位】：厦门大学材料学院;福建省海洋生物增养殖与高值化利用重点实验室福建省水产研究所;
【基金】：国家海洋局海洋公益性行业科研专项(No.201305043-4) 福建省省属公益类科研院所基本科研专项(No.2015R1003-7) 福建省海洋高新产业发展专项(闽海洋高新[2014]18号) 2014年第一批福建省地方标准制修订项目(闽质监标[2014]137号)资助
【分类号】：X830;O657.63

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