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超高效液相色谱-串联质谱法测定植物源食品中多抗霉素B、四霉素A和申嗪霉素残留量

Determination of residual levels of polyoxin B,tetramycin A and phenazine-1-carboxylic acid in foods of plant origin by ultra performance liquid chromatography-tandem mass spectrometry
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摘要 目的建立超高效液相色谱-串联质谱法测定植物源性食品中的多抗霉素B、四霉素A和申嗪霉素残留量的分析方法。方法样品采用乙腈提取,经HLB固相萃取柱净化,Waters BEH HILIC色谱柱分离,超高效液相色谱-串联质谱仪检测,基质匹配标准曲线外标法定量。结果多抗霉素B、四霉素A和申嗪霉素在5.0~200.0μg/L质量浓度范围内线性关系良好(r^(2)>0.995)。蔬菜、水果中多抗霉素B、四霉素A的定量限均为0.050 mg/kg,申嗪霉素的定量限为0.010 mg/kg。谷物中多抗霉素B、四霉素A的定量限为0.100 mg/kg,申嗪霉素的定量限为0.025 mg/kg。多抗霉素B在0.050~10.000 mg/kg添加水平回收率为80.5%~101.3%,相对标准偏差为0.72%~9.22%,申嗪霉素在0.010~10.000 mg/kg添加水平回收率为70.3%~108.2%,相对标准偏差为1.52%~9.80%,四霉素A在0.050~1.000 mg/kg添加水平回收率为80.4%~107.1%,相对标准偏差为1.45%~9.29%。结论本方法操作简单,准确性好,灵敏度高,可用于植物源性食品中多抗霉素B、四霉素A和申嗪霉素残留量的测定。 Objective To establish a method for the determination of polyoxin B,tetramycin A and phenazine-1-carboxylic acid residues in foods of plant origin by ultra performance liquid chromatography-tandem mass spectrometry.Methods The samples were extracted by acetonitrile,purified by Oasis PRiME HLB solid phase extraction column,separated by Waters BEH HILIC column,detected by ultra performance liquid chromatogue-tandem mass spectrometer,and quantified by matrix matching standard curve external standard method.Results The linear relationships of polyoxin B,tetramycin A and phenazine-1-carboxylic acid were good in the mass concentration range of 5.0-200.0μg/L(r^(2)>0.995).The limits of quantification of polyoxin B and tetramycin A in vegetables and fruits were 0.05 mg/kg,and those of phenazine-1-carboxylic acid were 0.010 mg/kg.The limits of quantification of polyoxin B and tetramycin A in cereals were 0.10 mg/kg,and those of phenazine-1-carboxylic acid were 0.025 mg/kg.The recoveries of polyoxin B supplemented with 0.050-10.000 mg/kg were 80.5%-101.3%,the relative standard deviations were 0.72%-9.22%,and the recoveries of phenazine-1-carboxylic acid supplemented with 0.010-10.000 mg/kg were 70.3%-108.2%,the relative standard deviations were 1.52%-9.80%.The recoveries of tetramycin A supplemented with 0.050-1.000 mg/kg were 80.4%-107.1%and the relative standard deviations were 1.45%-9.29%.Conclusion The method has the advantages of simple operation,good accuracy and high sensitivity,and can be used for the determination of polyoxin B,tetramycin A and phenazine-1-carboxylic acid residues in foods of plant origin.
作者 罗耀 黄科 赵凤娟 张建莹 赵旭 吴凤琪 张毅 黄刚 LUO Yao;HUANG Ke;ZHAO Feng-Juan;ZHANG Jian-Ying;ZHAO Xu;WU Feng-Qi;ZHANG Yi;HUANG Gang(Food Inspection&Quarantine Center,Shenzhen Customs,Shenzhen 518045,China;School of Materials and Environmental Engineering,Shenzhen Polytechnic University,Shenzhen 518055,China;Comprehensive Technology Center of Huizhou Customs,Huizhou 516006,China)
出处 《食品安全质量检测学报》 CAS 2024年第19期84-91,共8页 Journal of Food Safety and Quality
关键词 植物源 多抗霉素B 四霉素A 申嗪霉素 超高效液相色谱-串联质谱法 foods of plant origin polyoxin B tetramycin A phenazine-1-carboxylic acid ultra performance liquid chromatography-tandem mass spectrometry
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