高效液相色谱-串联质谱法检测鸡肉中金霉素、差向金霉素

Determination of chlortetracycline and 4-Epi-chlortetracycline in chicken muscle by liquid chromatography-tandem mass spectrometry

建立了高效液相色谱串联质谱(HPLC-MS/MS)快速测定鸡肉中差向金霉素、金霉素的检测方法。均质样品用pH4.0 EDTA-McIIvaine缓冲溶液提取,经Oasis HLB SPE小柱净化,采用LC-ESI-MS/MS和正离子多反应监测(MRM)模式检测。差向金霉素在0.025～0.8μg/mL,金霉素在0.005～0.2μg/mL浓度范围内线性关系良好,相关系数r均大于0.99。在0.05、0.10、0.15 mg/kg的加标水平下,回收率为73.0%～101.6%,相对标准偏差(RSD)为2.1%～12%。差向金霉素和金霉素的定量限分别为30.0、10.0μg/kg。该方法样品处理简单,可同时检测差向金霉素和金霉素的残留,且准确度和精密度均符合残留分析的要求。

A method was presented for the determination of 4-epi-chlortetracycline（ECTC） and chlortetracycline（CTC） by high performance liquid chromatography coupled with tandem quadrupole mass spectrometry（HPLC-MS/MS）.Samples were extracted with EDTA-McIlvaine buffer solution and cleaned up by Oasis HLB solid-phase extraction（SPE） column.The residues were detected by LC-ESI-MS/MS and the detection mode was multiple reaction monitoring with positive-ion electrospray ionization.The calibration curves were linear in a concentration range of 0.025~0.8 μg/mL for ECTC and 0.005~0.2 μg/mL for CTC with correlation coefficients more than 0.99.Recoveries of ECTC and CTC at fortified levels of 0.05、0.10、0.15 mg/kg ranged from 73.0% to 101.6%,with relative standard deviations of 2.1%~12%.The quantification limits are 30.0 μg/kg、10.0 μg/kg for ECTC and CTC,respectively.This method meets the demand for the determination of ECTC and CTC residues.