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目的建立测定蜂蜜中大观霉素、潮霉素B、链霉素、双氢链霉素和阿米卡星等5种氨基糖苷类药物残留量的液相色谱-串联质谱法(HPLC-MS/MS)。方法蜂蜜样品中的氨基糖苷类药物经磷酸盐缓冲液提取后,经过弱阳离子固相萃取柱富集净化后,采用液相色谱-三重四极杆串联质谱检测,使用电喷雾离子化源(ESI),在正离子条件下以多反应监测(MRM)方式进行扫描。采用异帕米星为内标进行定量分析。结果线性范围为10~1 000μg·kg-1,各被测物的最低定量浓度为0.6~5.2μg·kg-1;以加标样品计算,在各浓度水平下,各被测物的方法回收率为92.4%~103.2%;提取回收率为62.5%~81.6%。结论本方法准确、高效,适用于蜂蜜中氨基糖苷类药物残留量的检测。
OBJECTIVE To establish a liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of five aminoglycoside residues in honey including spectinomycin, hygromycin B, streptomycin, dihydrostreptomycin and amikacin MS). Methods The aminoglycosides in honey samples were extracted with phosphate buffer and purified by weak cation SPE column. The compounds were detected by liquid chromatography-triple quadrupole tandem mass spectrometry. Electrospray ionization (ESI ), Scanning in multiple reaction monitoring (MRM) mode under positive ion conditions. The use of ispamipin as internal standard for quantitative analysis. The linear range was 10-1 000 μg · kg-1, and the lowest concentration of each analyte was 0.6-5.2 μg · kg-1. The spiked samples were collected and spiked at various concentrations to recover the analytes The rates ranged from 92.4% to 103.2%. The extraction recoveries ranged from 62.5% to 81.6%. Conclusion The method is accurate and efficient and is suitable for the determination of aminoglycoside residues in honey.