建立了高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量的方法。样品经正己烷提取,苯并(a)芘分子印迹柱净化后,经Eclipse Plus C18色谱柱(150mm×4.6mm,5.0μm)分离,以体积分数为90%的乙腈溶液为流动相进行等度洗脱。结果表明:苯...建立了高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量的方法。样品经正己烷提取,苯并(a)芘分子印迹柱净化后,经Eclipse Plus C18色谱柱(150mm×4.6mm,5.0μm)分离,以体积分数为90%的乙腈溶液为流动相进行等度洗脱。结果表明:苯并(a)芘的质量浓度与其对应的峰面积在0.4~100μg·L^(-1)内呈线性关系,相关系数为0.9999。测定下限(10S/N)为0.40μg·kg^(-1)。以果蔬脆片样品为基质在3个浓度水平下进行加标回收试验,所得日内回收率为89.4%~93.7%,测定值的相对标准偏差(n=6)为4.3%~7.2%;日间回收率为87.6%~92.5%,测定值的相对标准偏差(n=6)为5.8%~8.4%。用此方法分析了20个果蔬脆片样品,在7个样品中检出了苯并(a)芘,但其含量均小于GB 2762-2017规定的限量(10μg·kg^(-1))。展开更多
[Objective]The research aimed to establish a liquid chromatography-high-resolution mass spectrometry for detecting residues of diclazuril,toltrazuril and its metabolites in animal-derived food.[Method]The samples were...[Objective]The research aimed to establish a liquid chromatography-high-resolution mass spectrometry for detecting residues of diclazuril,toltrazuril and its metabolites in animal-derived food.[Method]The samples were pre-treated by QuEChERS technology and detected by Exactive liquid chromatography-high resolution mass spectrometry.The liquid chromatography-high-resolution mass spectrometry for detecting the residues of diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food was established.[Result]Diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide showed a good linear correlation in the range of 2.0-50.0μg/L（r^2〉0.99）.The average recoveries of these four compounds in bovine power at the spiked levels of 2,10 and 20μg/kg were 74.5%-90.1%,and the relative standard deviations（RSD）were 15.4%-17.5%.[Conclusion]This method was stable and reliable,and could be used to detect diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food.展开更多
文摘建立了高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量的方法。样品经正己烷提取,苯并(a)芘分子印迹柱净化后,经Eclipse Plus C18色谱柱(150mm×4.6mm,5.0μm)分离,以体积分数为90%的乙腈溶液为流动相进行等度洗脱。结果表明:苯并(a)芘的质量浓度与其对应的峰面积在0.4~100μg·L^(-1)内呈线性关系,相关系数为0.9999。测定下限(10S/N)为0.40μg·kg^(-1)。以果蔬脆片样品为基质在3个浓度水平下进行加标回收试验,所得日内回收率为89.4%~93.7%,测定值的相对标准偏差(n=6)为4.3%~7.2%;日间回收率为87.6%~92.5%,测定值的相对标准偏差(n=6)为5.8%~8.4%。用此方法分析了20个果蔬脆片样品,在7个样品中检出了苯并(a)芘,但其含量均小于GB 2762-2017规定的限量(10μg·kg^(-1))。
基金Supported by Scientific Research Projects of General Administration of Quality Supervision,Inspection and Quarantine“Standard Sample Development and Production System Construction of Animal-derived Veterinary Drugs”(20130143)
文摘[Objective]The research aimed to establish a liquid chromatography-high-resolution mass spectrometry for detecting residues of diclazuril,toltrazuril and its metabolites in animal-derived food.[Method]The samples were pre-treated by QuEChERS technology and detected by Exactive liquid chromatography-high resolution mass spectrometry.The liquid chromatography-high-resolution mass spectrometry for detecting the residues of diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food was established.[Result]Diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide showed a good linear correlation in the range of 2.0-50.0μg/L（r^2〉0.99）.The average recoveries of these four compounds in bovine power at the spiked levels of 2,10 and 20μg/kg were 74.5%-90.1%,and the relative standard deviations（RSD）were 15.4%-17.5%.[Conclusion]This method was stable and reliable,and could be used to detect diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food.
