超高效液相色谱-串联质谱法测定水产品中群勃龙残留方法研究

Determination of trenbolone residues in fishery products by ultra performance liquid chromatography- tandem mass spectrometry

关键词:  水产品  群勃龙  残留  超高效液相色谱-串联质谱法

Key words:  trenbolone  fishery products  residues  UPLC-MS/MS

摘要:

建立了牛奶中苯并咪唑类药物及代谢物残留的超高效液相色谱-串联质谱检测方法。水产样品经乙酸乙酯提取，C18固相萃取柱净化，采用超高效液相色谱-串联质谱多反应监测模式检测，外标法定量。不同基质中，群勃龙在2 ng/mL～100 ng/mL的浓度范围内呈现良好的线性相关，相关系数为0.994以上；本方法对群勃龙群勃龙在鱼、虾、鳖、蟹类产品中的检测限为0.5μg/kg，定量限为1μg/kg；在贝类产品中的检测限为1μg/kg，定量限2μg/kg；不同水产品的基质中添加1礸/kg～10礸/kg浓度范围内，其回收率为74.2%～119%，批内变异系数在1.0%～9.0%之间，批间变异系数在0.3%～8.5%之间。本方法分析速度快，灵敏度高，重现性好，各项技术指标均满足国内外相关法规要求，可用于水产品中群勃龙的残留检测。

Abstract:

A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the determination of trenbolone residues in fishery products. The analyte was extracted with ethyl acetate, and cleaned by C18 solid phase extraction cartridge. Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) using external standard method. Detection Limits and quantification limits of this method for the analyte were all 0.5礸/g and 1礸/g in fish, shrimp, turtle, crab, and were 1礸/g and 2礸/g in seashell. The overall recovery varies from 74.2%～119% at the spiked level of 1礸/kg～10礸/kg in different sample, and the intra-and inter-batch coefficients was from 1.0%～9.0% and from 0.3%～8.5%, respectively. The method was reliable, sensitive and reproducibility, its performance can meet the requirements of the domestic and international legislation．The method adapts to the determination of trenbolone residues in fishery products.