为建立一种可同时检测鸽蛋中多类兽药残留的高通量液相色谱-串联质谱法,试验采用正己烷去脂,联合QuEChERS净化结合冷冻脂质过滤法,建立检测鸽蛋中5类24种兽药残留的高效液相色谱-串联质谱法.样品中的5类兽药(氯霉素类、磺胺类、硝基咪唑类、喹诺酮类和抗病毒类)经1.0%乙酸乙腈溶液提取,氮气吹干,冷冻过夜后,结合QuEChERS净化和正己烷去脂,采用1 mL 0.1%甲酸水-乙腈溶液(v/v,90∶10)复溶;高效液相色谱-串联质谱测定,内标法定量,采用实际样品建立方法的初步应用.结果显示:24种兽药在2.0～200 ng/mL线性关系良好(R2>0.99),该方法的定量限为2 μg/kg,平均回收率为62.2%～117.1%,相对标准偏差4.3%～18.9%;实际样品检出的7种目标化合物与标准方法相比的相对标准偏差为1.34%～5.20%.研究表明,建立的检测鸽蛋中多类兽药残留的高通量液相色谱-串联质谱法省去固相萃取步骤,成本较低,灵敏高效,回收率优良、重复性稳定,适用于鸽蛋中多类兽药的快速监测分析.
Simultaneous Determination of 5 Kinds of 24 Veterinary Drug Residues in Pigeon Eggs by Combined Purification Method Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry
To establish a method for the determination of veterinary drug residues in pigeon eggs by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),samples were extracted and purified using frozen lipid filtration combined with the QuEChERS method taking advantage of n-hexane liquid purification.A total of 24 veterinary drugs encompassing 5 classes of drug(chloramphenicols,sulfonamides,nitroimidazoles,quinolones and antiviral)in pigeon eggs were analyzed.The drugs were extracted in 1.0%acetic acid acetonitrile(v/v),dried with nitrogen and frozen at very low temperature.The drugs were diluted by mobile phases,and cleaned using frozen lipid filtration and n-hexane liquid purification.The separation of residue targets was performed with a gradient elution of 0.1%(v/v)formic acid aqueous solution and acetonitrile(v/v,90/10)as mobile phases and detected by HPLC-MS/MS by the internal standard method.The method was preliminarily applied with actual samples.The results showed that this method gave good linearity within a certain concentration range(R2>0.99),and the acceptable limit of quantification was 2.0 μg/kg,and the average recovery rate was from 62.2%to 117.1%,relative standard deviation was ranged from 4.3%to 18.9%for the 24 veterinary drugs.The relative standard deviations of 7 target compounds were from 1.34%to 5.20%compared with the standard method.The results indicated that the established HPLC-MS/MS proved suitable for the rapid determination of veterinary drugs residues in eggs with a simple,accurate,and low-cost procedure,and omitted the solid phase extraction.
combined purification methodhigh performance liquid chromatography-tandem mass spectrometryQuECh-ERSveterinary drug residuespigeon egg
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