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目的建立亲水高效液相色谱-串联质谱法测定蜂蜜中的链霉素。方法采用一种具有亲水作用的色谱柱(HILIC)(150mm×2.1mm,3.5μm),流动相为水(含5mmol/L醋酸铵和0.1%的甲酸)-乙腈(40:60)。样品经阳离子交换柱萃取净化,应用正离子电喷雾电离,MRM方式检测。结果方法的线性范围为10.5~105μg/kg,相关系数大于0.99,检出限为1.05μg/kg。加标回收率为71.3%~82.5%,RSD为3.4%~8.2%。结论该方法高效、灵敏、特异性强,准确度、精密度好,满足蜂蜜中链霉素的测定要求。
Objective To establish a method for the determination of streptomycin in honey by hydrophilic high performance liquid chromatography-tandem mass spectrometry. Methods A hydrophilic column (HILIC) (150 mm × 2.1 mm, 3.5 μm) was used. The mobile phase was water (containing 5 mmol / L ammonium acetate and 0.1% formic acid) -acetonitrile (40:60). Samples were purified by cation exchange column extraction, positive ion electrospray ionization, MRM detection. Results The linear range of the method was 10.5 ~ 105μg / kg, the correlation coefficient was greater than 0.99, and the detection limit was 1.05μg / kg. The spiked recoveries ranged from 71.3% to 82.5% with RSDs ranging from 3.4% to 8.2%. Conclusion The method is efficient, sensitive, specific, accurate and precise, which can meet the determination of streptomycin in honey.