混合型离子交换液相色谱-串联质谱法测定蜂蜜中5种氨基糖苷类抗生素残留

建立了混合型离子交换液相色谱-串联质谱测定蜂蜜中链霉素、双氢链霉素、壮观霉素、卡那霉素和阿米卡星等5种氨基糖苷类抗生素的方法。蜂蜜样品采用磷酸盐缓冲溶液提取,分子印迹固相萃取柱富集净化,Obelisc R色谱柱分离,以0.1%(v/v)甲酸水溶液和乙腈为流动相进行梯度洗脱,采用电喷雾电离、正离子模式扫描,多反应监测模式检测,外标法定量。实验结果表明,链霉素和双氢链霉素在5～100μg/L范围内呈现良好的线性关系,定量限为5μg/kg;壮观霉素、卡那霉素和阿米卡星在20～500μg/L范围内呈现良好的线性关系,定量限为20μg/kg。在空白蜂蜜样品中添加1倍、2倍和5倍定量限水平的5种氨基糖苷类药物,其平均回收率为75.1%～92.3%,相对标准偏差为4.5%～10.7%。该法不添加离子对试剂,可减少对质谱仪的污染,并具有较高的灵敏度,适用于蜂蜜中5种氨基糖苷类抗生素的同时检测。

Determination of five aminoglycoside residues in honey using mixed-mode ion exchange liquid chromatography-tandem mass spectrometry

A method using mixed-mode ion exchange liquid chromatography-tandem mass spectrometry was developed for the determination of streptomycin, dihydrostreptomycin, spectinomycin, kanamycin and amikacin in honey. The honey samples were extracted with phosphate followed by clean-up with SupelMIP Aminoglycosides SPE cartridges. The separation was performed on an SIELC Obelisc R column (100 mm×2.1 mm, 5 μm) by the gradient elution program using 0.1%(v/v) formic acid aqueous solution and acetonitrile as the mobile phases, at a flow rate of 0.4 mL/min. Five aminoglycosides (AGs) were identified by the tandem mass spectrometer with an electrospray ionization source under the multiple reaction monitoring (MRM) mode. The quantification analysis was performed by the external standard method. The calibration curves showed good linearity in the range of 5-100 μg/L for streptomycin and dihydrostreptomycin, and 20-500 μg/L for spectinomycin, kanamycin and amikacin. The limits of quantification (LOQs) of the five drugs in honey were 5-20 μg/kg. The average recoveries of the five drugs from feeds spiked at LOQ, 2-fold LOQ and 5-fold LOQ levels were 75.1%-92.3%, and the relative standard deviations (RSDs) were 4.5%-10.7%. The method is simple, rapid, and sensitive, and is suitable for the simultaneous determination of the five aminoglycoside residues in honey.