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

中文关键词:  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

英文关键词:Plant source  Polymycin B  Tetramycin A  Phenazine-1-carboxylic acid  Ultra high performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立一种超高效液相色谱-质谱/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，HILIC色谱柱分离，超高效液相色谱-质谱/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 μg/L浓度范围内线性关系良好（r2>0.99)。蔬菜、水果中多抗霉素B、四霉素A的定量限均为0.05 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0.10 mg/kg，申嗪霉素的定量限为0.025 mg/kg。多抗霉素B在0.05~10.0 mg/kg添加水平回收率为80.5%～101%，相对标准偏差为0.72%～9.22%，申嗪霉素在0.025~10.0 mg/kg添加水平回收率为70.3%～108%，相对标准偏差为1.52%～9.80%，四霉素A在0.05~1.0 mg/kg添加水平回收率为80.4%～107%，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。

英文摘要:

      Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of polyamycin B, tetramycin A and phenazine-1-carboxylic acid residues in plant-derived foods. Methods The samples were extracted by acetonitrile, purified by Oasis PRiME HLB solid phase extraction column, separated by Waters BEH HILIC column (2.1x100 mm, 1.7 μm), detected by ultra-high performance liquid chromatogue-tandem mass spectrometer, and quantified by matrix matching standard curve external standard method. Results The linear relationships of polyamycin B, tetramycin A and phenazine-1-carboxylic acid were good in the mass concentration range of 5.0~200 μg/L (r2>0.995). The limits of quantification of polyamycin 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 polyamycin 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 polyamycin B supplemented with 0.05-10.0 mg/kg were 80.5%-101%, the relative standard deviations were 0.72%-9.22%, and the recoveries of Shenazinomycin supplemented with 0.025-10.0 mg/kg were 70.3%-108%, the relative standard deviations were 1.52%-9.80%. The recoveries were 80.4%-107% and the relative standard deviations were 1.45%-9.29% when tetramycin A was added at 0.05-1.0 mg/kg. Conclusion The method is simple, accurate and sensitive, and can be used for the determination of polyamycin B, tetramycin A and phenazine-1-carboxylic acid residues in plant-derived foods.