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中国精品科技期刊2020
张敏,王鸽,马晓冲,等. 超高效液相色谱-串联质谱法测定牛乳中6种兽药残留[J]. 食品工业科技,2022,43(5):255−261. doi: 10.13386/j.issn1002-0306.2020110232.
引用本文: 张敏,王鸽,马晓冲,等. 超高效液相色谱-串联质谱法测定牛乳中6种兽药残留[J]. 食品工业科技,2022,43(5):255−261. doi: 10.13386/j.issn1002-0306.2020110232.
ZHANG Min, WANG Ge, MA Xiaochong, et al. Determination of 6 Kinds of Veterinary Drug Residues in Milk by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(5): 255−261. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020110232.
Citation: ZHANG Min, WANG Ge, MA Xiaochong, et al. Determination of 6 Kinds of Veterinary Drug Residues in Milk by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(5): 255−261. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020110232.

超高效液相色谱-串联质谱法测定牛乳中6种兽药残留

Determination of 6 Kinds of Veterinary Drug Residues in Milk by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

  • 摘要: 目的:建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定牛奶样品中6种兽药残留(硝碘酚腈、碘醚柳胺、氯氰碘柳胺、托曲珠利、三氯苯达唑、水杨酸钠)的检测方法。方法:样品经过乙腈溶液提取,以MAX固相萃取柱净化,采用Waters X Bridge BEH-C18色谱柱分离,流动相以乙腈和0.1%甲酸水溶液梯度洗脱,并使用电喷雾离子源,正负离子切换扫描模式进行检测,外标法定量。结果:6种兽药在0~10 ng/mL范围内呈现良好的线性关系,决定系数(R2)均大于0.995。6种兽药方法的检出限为0.06~0.18 μg/kg,方法的定量限为0.5~2.0 μg/kg。在添加量为0.5~8.0 μg/kg的加标回收实验下,6种兽药加标回收率为67.1%~105.5%,相对标准偏差均小于10%。结论:该方法前处理操作简便,分析速度快,灵敏度高,可用于牛奶样品中的兽药残留测定。

     

    Abstract: Objective: To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of six veterinary drug residues in milk samples. Methods: The sample was extracted with acetonitrile solution, purified with MAX solid phase extraction column, and separated by Waters X Bridge BEH-C18 chromatographic column. The mobile phase was eluted with a gradient of acetonitrile and 0.1% formic acid aqueous solution, and electrospray ion source was used, positive and negative ion switching scanning mode for detection, external standard method for quantification. Results: The 6 veterinary drugs showed a good linear relationship in the range of 0~10 ng/mL, and the coefficient of determination (R2) was greater than 0.995. The detection limit of the 6 veterinary drugs was 0.06~0.18 μg/kg. The limit of quantification of the method was 0.5~2.0 μg/kg. With the addition of 0.5~8.0 μg/kg in the standard recovery experiment, the recovery rates of the 6 veterinary drugs were 67.1%~105.5%, and the relative standard deviations were all less than 10%. Conclusion: This method is easy to operate, fast in analysis, and high in sensitivity. It can be used for the determination of veterinary drug residues in milk samples.

     

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