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| 高效液相色谱-串联质谱法测定鸡蛋中癸氧喹酯的残留 | |
| 引用本文： | 王中艳,罗浩师,张丽芳,江善祥,费陈忠,张可煜,郑文丽,王霄旸,薛飞群.高效液相色谱-串联质谱法测定鸡蛋中癸氧喹酯的残留[J].中国农学通报,2013,29(8):21-25. |
| 作者姓名： | 王中艳 罗浩师 张丽芳 江善祥 费陈忠 张可煜 郑文丽 王霄旸 薛飞群 |
| 作者单位： | 1. 中国农业科学院上海兽医研究所/农业部动物寄生虫病学重点实验室/中国农业科学院兽药安全评价与兽药残留重点开放实验室,上海200241;南京农业大学动物医学院/兽医药理与毒理实验室,南京210095 2. 中国农业科学院上海兽医研究所/农业部动物寄生虫病学重点实验室/中国农业科学院兽药安全评价与兽药残留重点开放实验室,上海,200241 3. 南京农业大学动物医学院/兽医药理与毒理实验室,南京,210095 |
| 基金项目： | 农业部2012年农业行业标准制修订项目 |
| 摘 要： | 为建立一种快速、灵敏的高效液相色谱-串联质谱法(LC-MS/MS)，以应用于癸氧喹酯(DEC)在鸡蛋中的残留检测，并将该方法用于残留消除规律的研究。将8只健康蛋鸡连续饲喂添加癸氧喹酯（浓度为27.2 mg/kg）的饲料10天后，分别在停药后第1、2、3、5、8、11天收集鸡蛋匀浆，用乙腈:乙酸乙酯(1:1)提取，OasisTM HLB固相萃取柱净化，以0.1%甲酸水:乙腈(30/70，v/v)作为流动相，XTerra C18色谱柱洗脱，质谱多反应监测(MRM)模式进行检测。结果表明：该方法的灵敏度高，检测限(LOD)和定量限(LOQ)分别为0.2、0.8μg/kg，DEC在0.8~240μg/kg浓度范围内线性良好，相关系数R2>0.993，回收率在90.7%~ 101.8%之间，RSD<11.4%；消除试验结果表明：鸡蛋中DEC最高残留浓度出现在停药后第3天，随着时间的推移，鸡蛋中癸氧喹酯的残留浓度逐渐降低，到第8天时该药的残留浓度达到欧洲委员会规定的允许浓度水平(20μg/kg)。本方法简便可靠，可满足检验实际需求。 |
| 关 键 词： | 耐热性 耐热性 |
| 收稿时间： | 5/4/2012 12:00:00 AM |
| 修稿时间： | 2012/12/25 0:00:00 |
Residue Determination of Decoquinate in Eggs by High Performance Liquid Chromatography-tandem Mass Spectrometry |
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| Abstract: | A rapid, sensitive and reliable high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the analysis of DEC in eggs, and the method has been successfully applied to the depletion study of DEC. The eight healthy laying hens fed medicated feed with decoquinate concentration of 27.2 mg/kg for 10 consecutive days. The egg samples were collected on days 1, 2, 3, 5, 8, 11 after the last dose and homogenized. The compound was extracted by acetonitrile-ethyl acetate using liquid-liquid extraction (LLE), and purified with OasisTM HLB Solid Phase extraction cartridge. Chromatographic separation was performed on an XTerra C18 reversed-phase column with a mobile-phase of water containing 0.1% formic acid and acetonitrile. The analyte was detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reaction monitoring (MRM). The results demonstrated that the method has high sensitivity with the LOD of 0.2μg/kg and the LOQ of 0.8μg/kg. The calibration curve showed good linearity with the concentrations of 0.8-240μg/kg with the correlation coefficient (R2>0.993). The recovery ranges from 90.7% to 101.8%, and RSD<11.4%. The result of depletion profile of DEC showed that the highest residue concentration of DEC was attained 3 days post-treatment. The residue concentration of DEC decreased to 20μg/kg which was the allowable concentration level of European Commission at 8 days after the last dose. The result showed that the method was rapid and reliable for application in practice. |
| Keywords: | residues elimination |
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