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中国精品科技期刊2020
乔勇升,王萍,黄银波,等. 固相萃取-超高效液相色谱-串联质谱同时测定乳制品中的苯并咪唑类药物及其代谢物残留量[J]. 食品工业科技,2024,45(13):1−9. doi: 10.13386/j.issn1002-0306.2023050242.
引用本文: 乔勇升,王萍,黄银波,等. 固相萃取-超高效液相色谱-串联质谱同时测定乳制品中的苯并咪唑类药物及其代谢物残留量[J]. 食品工业科技,2024,45(13):1−9. doi: 10.13386/j.issn1002-0306.2023050242.
QIAO Yongsheng, WANG Ping, HUANG Yinbo, et al. Simultaneous Determination of Benzimidazoles and Its Metabolites Residues in Dairy Products by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2024, 45(13): 1−9. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023050242.
Citation: QIAO Yongsheng, WANG Ping, HUANG Yinbo, et al. Simultaneous Determination of Benzimidazoles and Its Metabolites Residues in Dairy Products by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2024, 45(13): 1−9. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023050242.

固相萃取-超高效液相色谱-串联质谱同时测定乳制品中的苯并咪唑类药物及其代谢物残留量

Simultaneous Determination of Benzimidazoles and Its Metabolites Residues in Dairy Products by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了乳制品中苯并咪唑类药物固相萃取-超高效液相色谱-串联质谱的分析方法。样品经含0.2%甲酸的乙腈提取后离心,上清液使用固相萃取柱进行净化,UPLC HSS T3色谱柱分离,电喷雾正离子模式下多反应监测(Multiple Reaction Monitoring,MRM)测定。结果显示,在1.0~50 μg/L范围内的线性相关系数r≥0.995(除三氯苯达唑为0.9578),方法检出限(Limit of Detection,LOD)(S/N=3)为0.002 mg/kg(除阿苯达唑-2-氨基砜、噻苯达唑和噻苯咪唑-5-羟基为0.003 mg/kg),方法定量限(Limit of Quantitation,LOQ)(S/N=10)为0.005 mg/kg(除阿苯达唑-2-氨基砜、噻苯达唑和噻苯咪唑-5-羟基为0.010 mg/kg)。在0.005、0.01、0.05 mg/kg三个加标水平下回收率在62.5%~117.6%之间,相对标准偏差RSD在1.92%~12.17%之间。该方法操作简单、灵敏度高,适用于乳制品中苯并咪唑类药物及其代谢物的定量分析。

     

    Abstract: A method for the simultaneous determination of benzimidazoles and their metabolites in dairy products was established using ultra high performance liquid chromatography-tandem mass spectrometry (MS). After extracting the samples with acetonitrile containing 0.2% formic acid, the extracts were centrifuged and purified by solid phase extraction column, and then separated by UPLC HSS T3 chromatographic column, determined in multi reaction monitoring (MRM) method with a positive ESI mode. The results showed that the linear correlation coefficient (r) within the range of 1.0~50 μg/L was greater than 0.995 (except for trichlorophenyl-dazoxazole, which was 0.9578). The method had a limit of detection (LOD) of 0.002 mg/kg (except for albendazole-2-aminosulfone, thiabendazole, and thiabendazole-5-hydroxy, which were 0.003 mg/kg). The limit of quantitation (LOQ) (S/N=10) was 0.005 mg/kg (except for albendazole-2-aminosulfone, thiabendazole, and thiabendazole-5-hydroxy, which were 0.010 mg/kg). The recoveries at three spiked levels of 0.005, 0.01 and 0.05 mg/kg ranged from 62.5% to 117.6%, with relative standard deviations (RSD) between 1.92% and 12.17%. The method is simple to operate, highly sensitive, and suitable for the quantitative analysis of benzimidazoles and their metabolites in dairy products.

     

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