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中国精品科技期刊2020
谷悦,唐会鑫,李朔,等. QuEChERS-超高效液相色谱-三重四极杆串联质谱法测定水果制品和肉酱中10种四环素类抗生素[J]. 食品工业科技,2023,44(18):313−320. doi: 10.13386/j.issn1002-0306.2022100072.
引用本文: 谷悦,唐会鑫,李朔,等. QuEChERS-超高效液相色谱-三重四极杆串联质谱法测定水果制品和肉酱中10种四环素类抗生素[J]. 食品工业科技,2023,44(18):313−320. doi: 10.13386/j.issn1002-0306.2022100072.
GU Yue, TANG Huixin, LI Shuo, et al. Determination of 10 Tetracycline Antibiotics in Fruit Products and Meat Sauce by QuEChERS with Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(18): 313−320. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022100072.
Citation: GU Yue, TANG Huixin, LI Shuo, et al. Determination of 10 Tetracycline Antibiotics in Fruit Products and Meat Sauce by QuEChERS with Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(18): 313−320. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022100072.

QuEChERS-超高效液相色谱-三重四极杆串联质谱法测定水果制品和肉酱中10种四环素类抗生素

Determination of 10 Tetracycline Antibiotics in Fruit Products and Meat Sauce by QuEChERS with Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

  • 摘要: 使用QuEChERS结合超高效液相色谱-三重四极杆串联质谱(Ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry,UPLC-MS/MS),建立检测水果制品和肉酱中10种四环素类抗生素的分析方法。通过优化质谱参数、色谱条件和前处理技术,确定了最佳实验条件。样品经0.2%甲酸乙腈超声提取后,水果制品和肉酱分别用N-丙基乙二胺(PSA)和C18净化,经ZORBAX SB-Aq色谱柱(2.1 mm×150 mm,3.5 μm)分离,UPLC-MS/MS测定。结果显示,在各自线性范围内,10种四环素类抗生素具有良好的线性关系,相关系数(r)大于0.999;方法的检出限(LOD,S/N=3)为0.09~3.92 µg/kg,定量限(LOQ,S/N=10)为0.31~13.05 µg/kg;在75、300和750 µg/kg 3个不同加标水平下的平均回收率为70.0%~101.0%,相对标准偏差(Relative standard deviation,RSD)为1.0%~10.3%(n=7)。该方法灵敏、简便,适用于水果制品和肉酱中10种四环素类抗生素的快速同步检测。

     

    Abstract: A method for the determination of 10 tetracycline antibiotics in fruit products and meat sauce was established by QuEChERS coupled with ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS). The optimal experimental conditions were determined by optimizing the mass spectrometric parameters, chromatographic conditions and pre-treatment techniques. The samples were extracted by 0.2% formic acid acetonitrile under ultrasonication, and then purified with PSA for fruit products and C18 for meat sauce. The target analytes were separated on a ZORBAX SB-Aq column (2.1 mm×150 mm, 3.5 μm), and detected by UPLC-MS/MS. The results demonstrated that the 10 tetracycline antibiotics showed good linearity in the respective linear range with the correlation coefficients (r) higher than 0.999. The limits of detection (S/N=3) were 0.09~3.92 μg/kg, and the limits of quantification (S/N=10) were 0.31~13.05 μg/kg. The average recoveries at three different spiked levels of 75, 300 and 750 μg/kg ranged from 70.0% to 101.0% with the relative standard deviation (RSD) of 1.0%~10.3% (n=7). The method is sensitive, simple and suitable for the rapid and simultaneous detection of 10 tetracycline antibiotics in fruit products and meat sauce.

     

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