液相色谱—串联质谱法测定猪可食用组织中氨茶碱残留
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(1. 唐山市食品药品综合检验检测中心,河北 唐山 063000;2. 河北省农产品质量安全检测工程技术创新中心,河北 唐山 063000)

作者简介:

张丽芳,女,唐山市食品药品综合检验检测中心高级农艺师,硕士。

通讯作者:

周鑫(1982—),男,唐山市食品药品综合检验检测中心正高级兽医师,硕士。E-mail: 122750039@qq.com

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基金项目:

唐山市科技计划项目(编号:22150220A);唐山市科技创新领军人才项目(编号:21130243A);唐山市人才资助项目(编号:A202110013)


Determination of aminophylline residues in edible tissues of pig by high performance liquid chromatography tandem mass spectrometry
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(1. Tangshan Food and Drug Comprehensive Testing Center, Tangshan, Hebei 063000, China; 2. Hebei Agricultural Products Quality and Safety Testing Innovation Center, Tangshan, Hebei 063000, China)

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    摘要:

    目的:研究猪可食用组织中氨茶碱药物残留的定性定量测定方法。方法:建立固相萃取净化结合高效液相色谱—串联质谱法,试样中的氨茶碱药物残留被甲醇溶液提取后,经PRiME HLB固相萃取柱一步净化,随后用C18色谱柱分离,以0.1%甲酸水溶液和乙腈分别作为水相和有机相对氨茶碱进行色谱柱梯度洗脱,利用电喷雾正电压离子化并采用多反应监测模式进行化合物检测,空白基质匹配标准曲线外标法定量。结果:氨茶碱药物在3.5 min内完成仪器分析,不同基质的匹配曲线在0.005~0.1 μg/mL质量浓度范围内呈良好的线性关系(R>0.998 0),猪肉、猪肝、猪肾的方法加标平均回收率为87.2%~101.3%,相对标准偏差为0.7%~6.2%(n=6),方法检出限为2 μg/kg,定量限为5 μg/kg。结论:该方法简便高效、重复性好、灵敏度高,适用于猪的可食用组织中氨茶碱药物残留的定性定量分析。

    Abstract:

    Objective: A method for the determination of aminophylline residues in edible tissues (muscle, liver and kidney) of pigs by solid-phase extraction combined with high performance liquid chromatography-tandem mass spectrometry was established. Methods: After extracted by methanol, the aminophylline was purified by PRiME HLB solid phase extraction column in one step, and then separated by a C18 chromatographic column. 0.1% formic acid solution and acetonitrile were invoked as the aqueous phase and the organic phase for gradient elution, respectively. Electrospray positive voltage ionization and multi reaction monitoring (MRM) mode are used for compound detection, and matrix matching standard was used for quantification. Results: The analysis of aminophylline drugs was completed within 3.5 minutes, and the results showed good linear relationship (R>0.998 0) on different matrices in the concentration range of 0.05~1.0 μg/mL. The average recoveries ranged from 87.2% to 101.3%, and the relative standard deviations ranged from 0.7% to 6.2% (n=6). The detection limit was 2 μg/kg and the quantification limit was 5 μg/kg. Conclusion: The method which is simple and efficient, has good repeatability and high sensitivity. It is suitable for qualitative and quantitative analysis of aminophylline drug residues in edible tissues of pigs.

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张丽芳,肖 琎,李 宁,等.液相色谱—串联质谱法测定猪可食用组织中氨茶碱残留[J].食品与机械,2023,39(7):62-67.
ZHANG Li-fang, XIAO Jin, LING Ning, et al. Determination of aminophylline residues in edible tissues of pig by high performance liquid chromatography tandem mass spectrometry[J]. Food & Machinery,2023,39(7):62-67.

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  • 收稿日期:2022-09-09
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  • 在线发布日期: 2023-10-20
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