高效液相色谱-串联质谱法测定蜂蜜中10种氨基糖苷类药物  

Detection of 10 Aminoglycosides Drugs in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孙婷 沈鹭英 何金麟 占永超 严丽娟 徐敦明 SUN Ting;SHEN Lu-ying;HE Jin-lin;ZHAN Yong-chao;YAN Li-juan;XU Dun-ming(Xiamen Customs Technology Center,Xiamen 361026,China)

机构地区：[1]厦门海关技术中心,福建厦门361026

出　　处：《分析测试学报》2024年第7期1046-1051,1057,共7页Journal of Instrumental Analysis

基　　金：国家重点研发计划项目(2023YFF1104900);福建省自然科学基金(2023J01187)。

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)检测蜂蜜中10种氨基糖苷类药物(安普霉素、庆大霉素C1、卡那霉素、潮霉素B、巴龙霉素、阿米卡星、依替米星、奈替米星、妥布霉素和核糖霉素)残留量的方法。蜂蜜样品采用100 mmol/L磷酸盐缓冲液(pH 8.0)提取,SupelMIP SPE-Aminoglycosides分子印迹聚合物固相萃取柱净化,Thermo Hypercarb色谱柱分离,以5%氨水和乙腈为流动相进行梯度洗脱,采用HPLC-MS/MS电喷雾正离子模式检测,基质匹配标准曲线外标法定量。结果表明,10种氨基糖苷类药物在20~500μg/L范围内线性关系良好,方法定量下限为25μg/kg。在25、50、250μg/kg 3个加标水平下,10种氨基糖苷类药物的平均回收率为73.4%~93.2%,相对标准偏差(RSD)为5.2%~11%。该方法简便、灵敏度高,无需离子对试剂,有效减少了对质谱仪的污染,能够较好地满足蜂蜜中氨基糖苷类药物残留量的检测需要。A method was established for the detection of residues of ten aminoglycoside(AGs)drugs(apramycin,gentamycin C1,kanamycin,hygromycin B,paromomycin,amikacin,etimicin,netimicin,tobramycin and ribostamycin)in honey using high performance liquid chromatography-tan⁃dem mass spectrometry(HPLC-MS/MS).Several conditions were optimized,including sample ex⁃traction and purification,chromatographic conditions and mass spectrometry parameters.The honey samples were extracted with 100 mmol/L phosphate buffer(pH 8.0)and purified with SuperMIP SPE column.The eluent was 1.0 mL acetonitrile water(20∶80,volume ratio)solution containing 5%for⁃mic acid.Furthermore,the chromatographic separation conditions and response intensities of the 10 AGs in different mobile phases were compared.The optimized HPLC conditions were as follows:Thermo Hypercarb chromatography column(150 mm×2.1 mm,5μm);column temperature,35℃;flow rate,0.35 mL/min;injection volume,10μL;mobile phase A:5%ammonia solu⁃tion;mobile phase B:acetonitrile.The samples were quantified using positive-ion multiple reaction monitoring(MRM)mode for 13 min.The AGs were quantified using an external standard with matrix calibration curves to reduce the influences of the matrix effects on the quantitative results.The cali⁃bration curves showed good linearity in the range of 20-500μg/L,and the limits of quantification(LOQs)of ten aminoglycoside drugs in honey were 25μg/kg.The recoveries for the analytes at three spiked levels(25,50,250μg/kg)ranged from 73.4%to 93.2%,with relative standard deviations(RSDs)of 5.2%-11%.The method is simple,highly sensitive,and avoids the use of ion pair re⁃agents throughout the process,effectively reducing contamination of the mass spectrometer and it is suitable for detection of aminoglycosides in honey.

关 键 词：氨基糖苷类药物 高效液相色谱-串联质谱 分子印迹固相萃取 蜂蜜 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]