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[目的]建立一种使用液相色谱-串联质谱联用仪快速准确检测池塘沉积物中痕量氯霉素残留的方法,为水产品中氯霉素污染来源的排查提供技术支持。[方法]底泥经润湿后,经乙酸乙酯水饱和溶液提取,Sep-Pa K C_(18)固相萃取柱净化,Shim-Pack XR-ODS色谱柱分离,采用甲醇和水为流动相,并用梯度洗脱对待测物进行分离,以氘代氯霉素(氯霉素-D5)为内标,采用负离子扫描,多反应监测模式(MRM),定性离子对m/z为321→152.0,256.8,定量离子对m/z为321→152.0。[结果]氯霉素类药物在0.5~10.0 ng/m L范围内线性良好,相关系数均大于0.99,本方法的检出限为0.1μg/kg,定量限为0.3μg/kg。3个加标水平(0.5、1.0和5.0μg/kg)的平均回收率为90.1%~96.6%,相对标准偏差为2.4%~7.0%。[结论]实验结果符合氯霉素药物残留检测的相关法规要求,适用于淡水池塘沉积物中氯霉素残留的定性定量检测。
[Objective] The research aimed to establish a rapid and accurate method for the determination of trace chloramphenicol residues in pond sediment by using liquid chromatography-tandem mass spectrometry, and provide technical support for the investigation of the source of chloramphenicol pollution in aquatic products. [Method] The sediment was wetted, extracted with saturated aqueous solution of ethyl acetate, purified with Sep-Pa K C 18 solid phase extraction column and separated on a Shim-Pack XR-ODS column. The mobile phase consisted of methanol and water , And the analytes were separated by gradient elution. The deuterium chloramphenicol (chloramphenicol-D5) was used as internal standard, and negative ion scan and multi-reaction monitoring mode (MRM) were used. The qualitative ion pair m / z was 321 → 152.0 , 256.8, quantitative ion pair m / z 321 → 152.0. [Results] The linearity of chloramphenicol in the range of 0.5-10.0 ng / mL was good with the correlation coefficients greater than 0.99. The detection limit of this method was 0.1 μg / kg and the limit of quantification was 0.3 μg / kg. The average recoveries at three spiked levels (0.5, 1.0 and 5.0 μg / kg) ranged from 90.1% to 96.6% with relative standard deviations of 2.4% to 7.0%. [Conclusion] The experimental results accorded with the relevant regulatory requirements of chloramphenicol drug residue detection and was suitable for qualitative and quantitative detection of chloramphenicol residues in freshwater pond sediments.