摘要
目的建立一种专属、灵敏的液相色谱-串联质谱法(LC-MS/MS)测定蜂蜜中链霉素和双氢链霉素的残留量。方法用磷酸盐缓冲溶液提取蜂蜜中的链霉素和双氢链霉素后,经弱阳离子交换柱(WCX)进行固相萃取,样品制备后采用亲水作用色谱(HILIC),使链霉素和双氢链霉素实现保留,从而与内源性物质达到分离,采用电喷雾离子化串联质谱法(ESI-MS/MS)检测和定量。双氢链霉素的同位素离子较链霉素大3个质量单位,以此为母离子可有效减少或避免二者之间的光谱重叠现象。结果蜂蜜中链霉素和双氢链霉素的最低定量限(LLOQ)分别为0.5μg/kg和1.0μg/kg。结论该HILIC-MS/MS法灵敏、专属,适用于监测和分析蜂蜜中链霉素和双氢链霉素的残留量。
Objective A specific and sensitive liquid chromatography-tandem mass spectrometry （LC-MS/ MS） method was developed to determine streptomycin and dihydrostreptomycin residues in honey. Methods Streptomycin and dihydrostreptomycin were extracted from honey samples using a liquid extraction with a phosphate buffer followed by a solid-phase extraction based on weak cation-exchange （WCX） columns. After sample preparation, the hydrophilic interaction chromatography （HILIC） was used to retain streptomycin and dihydrostreptomycin on the column for the separation of the analytes from endogenous compounds. The aminoglycosides were detected and quantified with electrospray ionization tandem mass spectrometry （ESI-MS/MS）. To decrease or avoid effectively the spectra overlap of streptomycin and dihydrostreptomycin, isotopologue ion of the latter was used as parent ion, which differed 3 mass units from the former. Results The lower limits of quantification （ LLOQ ） of streptomycin and dihydrostreptomycin in honey were 0.5μg/kg and 1.0 μg/kg, respectively. Conclusion This HILIC-MS/MS method is sensitive and specific to monitor and analyze of streptomycin and dihydrostreptomycin residues in honey.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2009年第11期669-677,共9页
Chinese Journal of Antibiotics
关键词
液相色谱-串联质谱法
亲水作用色谱
链霉素
双氢链霉素
蜂蜜
Liquid chromatography-tandem mass spectrometry
Hydrophilic interaction chromatography
Streptomycin
Dihydrostreptomycin
Honey
