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为建立溴硝醇在草鱼肌肉组织中的残留检测方法,实验对比了草鱼肌肉样品经四种不同复合提取剂提取、正己烷去脂,4 500 r/min高速离心过滤膜后的回收效果,利用超高效液相色谱—质谱串联法(ultra-high performance liquid chromatography coupled with tandem mass spectrometry,UPLC-MS/MS)建立了溴硝醇在草鱼肌肉组织中的残留检测方法。结果表明复合沉淀剂OR-1801是前处理时效果最优提取剂;研究建立的残留检测方法在0～8 mg/kg的浓度范围内线性良好,标准曲线方程为Y=17 652.0X,回归系数r2=0.998;方法灵敏度高,检测限达0.1 mg/kg,定量限达0.25 mg/kg;根据0.5 mg/kg、2 mg/kg、4 mg/kg三个添加浓度进行回收实验,检测方法重复性好,平均回收率范围为87.7%～100.8%,变异系数范围为2.0%～5.4%。本研究解决了溴硝醇在草鱼肌肉组织中不易提取的难题,首次建立了草鱼肌肉中溴硝醇的残留检测方法,满足对草鱼等水产品肌肉组织中的溴硝醇残留定性、定量检测要求,可为水产品的食品安全监控提供技术参考。
Abstract：To establish a method for detecting the residue of bronopol in muscle of grass carp. The effects of the reclaiming by four different compound extractants, de-lipidation with n-hexane, filtrated membrane after highspeed centrifugal at 4 500 r/min were compared. The ultra-high performance liquid chromatography-mass spectrometry was used to establish the method. The results showed that the composite precipitant OR-1801 was the best extractant for the extraction of bronopol in grass carp muscle. The residue detection method established in the study had good linearity at the concentration range of 0～8 mg/kg, the standard curve equation is Y=17 652.0 X, and the regression coefficient r2=0.998. The method had high sensitivity with the limitation of detection from 0.1 mg/kg to2.5 mg/kg. The recovery experiments were carried out with bronopol added at the concentration of 0.5 mg/kg, 2 mg/kg and 4 mg/kg. The method has a good recovery range of 87.7%～100.8% with the coefficient of variation varies from2.0% to 5.4%. which also had good repeatability. This study solved the problem that bronopol is difficult to extract in the muscle tissue of grass carp. The residue detection method meets the demands of the detection and quantifying for the residues of bronopol in aquatic animals such as grass carp which also provided a technical reference in monitoring aquatic animal food safety.
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基本信息:
DOI：10.13417/j.gab.039.004910
中图分类号:O657.63;TS254.7
引用信息:
[1]孙晶,郑瑞州,王雅丽,等.利用UPLC-MS/MS检测草鱼中溴硝醇残留方法的建立[J].基因组学与应用生物学,2020,39(11):4910-4917.DOI:10.13417/j.gab.039.004910.
基金信息:
上海市地方高校能力提升项目(17050502100);; 上海市科委项目(18391901500)共同资助
2020-03-10
2020-03-10
2020-03-10