HPLC-MS/MS测定蜂蜜中氨基糖苷类药物残留

Residue Determination of Aminoglycosides in Honey by HPLC-MS/MS

关键词:  氨基糖苷  液相色谱-串联质谱  残留检测  蜂蜜

Key words:  aminoglycosides  LC–MS/MS  residue  honey

摘要:

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10~1 000 μg·kg^-1，各被测物的最低定量浓度为0.6~5.2 μg·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。

Abstract:

OBJECTIVE To develop a specific and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the residue determination of spectinomycin, hygromycin B, streptomycin, dihydrostreptomycin and amikacin in honey. METHODS After extraction of these analytes from honey samples with a phosphate buffer, the extract was loaded on a weak cation-exchange (WCX) solid-phase extraction column. After sample preparation, the hydrophilic interaction chromatography (HILIC) was used to retain the aminoglycosides on the column for the separation of the analytes from endogenous compounds. The aminoglycosides were detected and quantified with triple quadrupole tandem mass spectrometry with ESI source in the positive ion mode. Quantitation was performed using multiple reaction monitoring (MRM) of the transitions with isepamycin as the internal standard. RESULTS The linear regressions were fitted over the concentration range of 10-1 000 μg·kg^-1 for the analytes in honey. The lower limit of quantification of the analytes were all in 0.6-5.2 μg·kg^-1. The method and extracted recoveries of the analytes evaluated by determining the spiked samples at all levels were 92.4%-103.2% and 62.5%-81.6%, respectively. CONCLUSION The developed LC-MS/MS method is accurate and efficient enough to determine aminoglycosides in honey.