优化高效液相色谱-串联质谱法检测水产品中酰胺醇类药物残留

目的:对GB/T 20756—2006水产品中酰胺醇类残留量的测定方法进行了优化。方法:经匀质的水产品样品,加10 mL乙腈涡旋振荡,一次提取和除杂后,取4 mL提取液,35℃水浴氮吹近干,用20%乙腈水1 mL定容,过0.22 μm滤膜。样液用高效液相色谱进行分离,电喷雾串联四级杆质谱进行检测,以氯霉素-D5为内标物进行定量。结果:本次试验的线性范围在0.10～6.00 μg·kg^-1,相关系数均大于0.999,方法的回收率为83.2%～93.6%,相对标准偏差在2.7%～9.9%。结论:该方法灵敏度高,准确性好,与GB/T 20756—2006相比,简化了前处理步骤,回收率稳定。通过验证,该方法适用于开展水产品中酰胺醇类残留的检测。

Optimization of High Performance Liquid Chromatography-Tandem Mass Spectrometry for the Detection of Amide Alcohol Drug Residues in Aquatic Products

Objective:to optimize the method for the determination of amidol residues in aquatic products(GB/T 20756—2006).Methods:The homogenized aquatic product sample was added with 10 mL acetonitrile for vortex oscillation,followed by primary extraction and impurity removal.Then 4 mL of the extractive solution was taken,blown nearly dry under nitrogen in a 35℃water bath,fixed in volume with 1 mL of 20%acetonitrile water,and passed through a 0.22μm filter membrane.The sample was separated by high performance liquid chromatography(HPLC)and detected by electrospray ionization tandem mass spectrometry with chloramphenicol-D5 as the internal standard for quantification.Results:The linear range of the method was from 0.10μg·kg^-1 to 6.00μg·kg^-1,the correlation coefficients are all greater than 0.999.The recovery of the method was in the range of 83.2%~93.6%,and the relative standard deviation was in the range of 2.7%~9.9%.Conclusion:This method has the advantages of high sensitivity and good accuracy.Compared with GB/T 20756—2006,the pre-treatment steps were simplified and the recovery rate was stable.Through verification,the method is suitable for the detection of amide alcohol residues in aquatic products.