超高效液相色谱-串联质谱法测定土壤中多种兽用抗生素残留

李晓晶; 于鸿; 甘平胜

doi:10.13421/j.cnki.hjwsxzz.2016.04.009

超高效液相色谱-串联质谱法测定土壤中多种兽用抗生素残留

Determination of Antibiotic Residues in Soil by UPLC-MS/MS

摘要

摘要:
目的建立土壤中喹诺酮类、大环内酯类、林可霉素兽用抗生素超高效液相色谱-串联质谱（UPLC-MS/MS）快速分析方法。
方法样品用V（乙腈）：V（含0.1 mol/L EDTA的磷酸盐pH=9.0缓冲溶液）为1:1提取液超声提取，SAX-HLB串联固相萃取柱净化，C₁₈超高效色谱柱分离，采用串联质谱电喷雾离子源（ESI），在多反应监测正离子模式下测定，外标法定量。
结果加标水平为5.0 μg/kg、10 μg/kg、40 μg/kg时，回收率均在65.2%~106.5%之间，相对标准偏差2.4%~14.4%。方法在5 μg/L~100 μg/L的浓度范围内呈良好线性关系，线性相关系数大于0.9971，检测限为0.24 μg/L~2.90 μg/kg。
结论方法适用于土壤样品中多种抗生素的同时定量检测。

Abstract:
Objective To develop a fast ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) to determine Quinolones, Macrolides and Lincomycins residues in soil.
Methods Samples were extracted ultrasonically by V (1:1 aeetonitrile and 0.1 mol/L EDTA) and purified by SAX and HLB tandem solid phase extraction column, separated by ultra-performance chromatography column C₁₈, analyzed by using tandem mass spectrometry electrospray ion source under multiple reaction monitoring positive ion mode, and quantified by external standard.
Results The average recovery in the addition of standard at 5.0 μg/kg, 10 μg/kg and 40 μg/kg was in the range of 65.2%~106.5%, and the relative standard deviation was in the range of 2.4%~14.4%.The linearity was satisfactory with a correlation coefficient of >0.9971 in the concentration of 5 μg/L~100 μg/L. The limit of quantification (LOQ) was 0.24 μg/kg~2.90 μg/kg.
Conclusion The method was suitable for quantitative analysis and confirmation of antibiotic residues in soil

HTML全文

参考文献(6)

施引文献

资源附件(0)