Detection of nine aminoglycosides residues in honey by ultra-performance liquid chromatography-tandem mass spectrometry
MA Kai1, CAI Fangye2, HUANG Yongqiao1, WU Xinwen1, YANG Changbiao1, LI Zhanbin1*
1(Guizhou Academy of Testing and Analysis, Guiyang 550000, China) 2(Shenqi Ethnic Medicine College of Guizhou Medical University, Guiyang 550000, China)
Abstract: Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous detection of aminoglycosides (neomycin, amikacin, dihydrostreptomycin, streptomycin, hygromyxin B, kananmycin, gendamicin, tobramycin, spectinomycin). The residues of aminoglycosides in the honey were extracted with TCA buffer, enriched and cleaned up with HLB solid phase extraction column, and eluted with aqueous elution. And the ion-pairing reagent was added to the final extract and used to optimize the chromatography conditions. Moreover, the extracts were separated on reversed-phase chromatographic column using acetonitrile-water as mobile phase by gradient elution, and detected by liquid chromatography-mass spectrometry under multiple reaction monitoring mode via positive ion mode. All the analytes were calibrated by the external method. The results showed that the method has a good linear relationship in the range of 20-1 000 ng/mL. Moreover, the quantification limit of neomycin, dihydrostreptomycin, streptomycin, kanamycin, and tobramycin is 5 μg/kg; the quantification limit of amikacin, hygromycin B, gentamicin, and spectinomycin is 10 μg/kg. Within the linear range, three concentrations of addition experiments were carried out in the blank honey samples, the sample recovery rates ranged from 72.6%-109.4%, and the relative standard deviations were 2.13%-8.23%. The method developed here has the advantages of easy operation, high sensitivity and good filter effect. By avoiding the use of ion-pairing reagent in the mobile phase, the method could effectively reduce the pollution of mass spectrometer and better meet the detection requirements of the aminoglycoside residues in honey.
马凯,蔡芳叶,黄永桥,等. 超高效液相色谱-串联质谱法检测蜂蜜中九种氨基糖苷类药物残留[J]. 食品与发酵工业, 2020, 46(18): 203-208.
MA Kai,CAI Fangye,HUANG Yongqiao,et al. Detection of nine aminoglycosides residues in honey by ultra-performance liquid chromatography-tandem mass spectrometry[J]. Food and Fermentation Industries, 2020, 46(18): 203-208.
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2020, Vol. 46 
