超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定牛奶中19种喹诺酮类抗生素
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“十三五”国家重点研发计划重点专项(2018YFC1603400); 河北省科技计划项目(19225503D)


Determination of 19 Kinds of Quinolones in Milk by Ultra Performance Liquid Chromatography/ Quadrupole Obitrap High Resolution Mass Spectrometry
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    摘要:

    建立基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱筛查和确证牛奶中19种喹诺酮类抗生素的方法。牛奶样品经酸化乙腈提取并沉淀蛋白,PRiME HLB固相萃取柱净化,用Waters Acquity BEH C_(18)柱(2.1 mm×100 mm,2.5μm)分离,以乙腈和0.1%甲酸水溶液进行梯度洗脱,在全扫描(full MS)-数据依赖扫描(ddMS~2)模式下检测。结果表明:19种喹诺酮类抗生素的精确质量相对偏差小于3.0×10~(-6),在0.2~200 ng/mL范围线性关系良好;检出限0.1~0.5μg/kg,定量限0.2~1.0μg/kg;加标水平0.2~10.0μg/kg时,方法回收率62.1%~100.4%,相对标准偏差低于10%。该方法简便、快速、准确,适用于牛奶中19种喹诺酮类抗生素的快速筛查和定量分析。

    Abstract:

    A rapid method was presented for the determination of 19 quinolone antibiotics in milk by ultra high performance liquid chromatography/ quadrupole orbitrap high resolution mass spectrometry. Milk samples were extracted by acidified acetonitrile and purified by PRiME HLB solid phase extraction column, then separated by Waters Acquity BEH C18 column (100 mm×2.1 mm, 2.5 μm) using a binary solvent system composed of acetonitrile and water(0.1% formic acid) by gradient elution. The analytes were determined by quadrupole-orbitrap high resolution mass spectrometry in full-MS and data-dependent scan (ddMS2) mode. The results showed that mass accuracy error of the 19 quinolones were lower than 3.0×10-6, linear relationships were well in the range of 0.2-200 ng/mL for 19 antibiotics, and correlation coefficients were higher than 0.998. The LODs were in the range of 0.1-0.5 μg/kg and the LOQs were in the range of 0.2-1.0 μg/kg. With spike levels in the range of 0.2-10.0 μg/kg, recovery of the method was in range of 62.1%-100.4% and relative standard deviations were lower than 10%. The method is simple, rapid, accurate, which is suitable for the rapid screening and quantitative analysis of 19 kinds of quinolones antibiotics in milk sample.

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马俊美;范素芳;孙磊;张明星;张冬生;李强;.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定牛奶中19种喹诺酮类抗生素[J].中国食品学报,2021,21(1):309-317

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  • 在线发布日期: 2021-02-22
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