亲水高效液相色谱-串联质谱法测定蜂蜜中的链霉素

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。

Determination of streptomycin in honey determined by hydrophilic interaction chromatography combined with tandem mass spectrometry

Objective To establish a method for the determination of streptomycin in honey by determined hydrophilic interaction chromatography combined with tandem mass spectrometry ( HILIC-MS/MS). Methods A hilic column was used, and the mobile phase was consisted of acetonitrile (5 mmol/L ammonium acetate and 0. 1 % formic acid, 60:40 ). Samples were extracted by the cation-exchange SPE cartridge. The extraction samples were then identified and quantitated by HILIC-ESI-MS/MS. Results Linear calibration curves were obtained at the concentration ranges from 10. 5 μg/kg to 105 μg/kg (the correlation coefficients were above 0. 99 ). The limit of detection was 1. 05 μg/kg. The average recoveries for streptomycin spiked in honey ranged from 71. 3 to 82. 5% and their relative standard were between 3.4% and 8. 2% . Conclusion The method for determination of streptomycin in honey could be simple, sensitive and accurate.