亲水性ObeliscR液相色谱-串联质谱法测定猪肉样品中氨基糖苷类药物残留  

Determination of Aminoglycosides Residue in Pork by Hydrophilic Obelisc R Column-HPLC-MS/MS

作　　者：赵凤娟[1] 方恩华 韩瑞阳[1] 彭毅候 罗耀[1] 熊贝贝[1] 蔡伊娜[1] 李丽苏[1] ZHAO Fengjuan;FANG Enhua;HAN Ruiyang;PENG Yihou;LUO Yao;XIONG Beibei;CAI Yina;LI Lisu(Food Inspection and Quarantine Center, Shenzhen Entry Exit Inspection and Quarantine Bureau,Shenzhen Key Laboratory of Detection Technology R&D on Food Safety,Shenzhen518045,China;Xiamen Entry Exit Inspection and Quarantine Technology Center,Xiamen361026,China)

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,深圳市食品安全检测技术研发重点实验室,广东深圳518045 [2]厦门出入境检验检疫局检验检疫技术中心,福建厦门361026

出　　处：《质谱学报》2018年第1期76-84,共9页Journal of Chinese Mass Spectrometry Society

基　　金：国家质检总局科技项目(2015IK250)资助

摘　　要：建立了高效液相色谱-串联质谱法测定猪肉中9种氨基糖苷类药物(壮观霉素、潮霉素B、双氢链霉素、链霉素、阿米卡星、卡那霉素、安普霉素、妥布霉素、庆大霉素)残留量。待测样品中的氨基糖苷类药物经磷酸盐缓冲溶液提取,调节pH值后,经SupelMIP~ SPE-Aminoglycosides分子印迹固相萃取柱净化、浓缩、定容,然后采用Obelisc R高效液相色谱柱分离,以串联质谱法正离子模式检测。该方法在20~1 000μg/L范围内线性关系良好。在线性范围内,分别进行高、中、低3个浓度的添加实验,样品的回收率在76.9%~89.4%之间,相对标准偏差在3.56%~11.4%之间。该方法简便、快速、准确,可以满足猪肉中氨基糖苷类药物残留的测定需求。The molecular structure and physicochemical property of common aminoglycosides(AGs)antibiotics were systematically analyzed and the residue of animal origin foodstuffs as well as the corresponding damage on human body with long-term intake were introduced.Concrete ideas of the study were raised based on the analysis of present analytical approaches and the discussion of existing defects.An HPLC-MS/MS analytical method was developed for the simultaneous determination of aminoglycosides(spectinomycin,hygromycin B,dihydrostrepmycin,streptomycin,amkacin,kanamycin,apramycin,tobramycin,gentamicin)with a new hydrophilic HPLC column.The residues of aminoglycosides in the test samples were extracted with phosphate buffer solution.After ajusting pH values,the samples were cleaned up with SupelMIP SPE column,concentrated and reconstituted,the residues were separated by Obelisc R HPLC column(2.1mm×150mm×5μm,100A)by gradient elution with acetonitrile water(1%formic acid)as mobile phase,and detected by liquid chromatography mass spectrometry under multiple reaction monitoring(MRM)mode via positive ion mode.All the analytes were calibrated by the external method.The matrix effects were evaluated by comparing solvent prepared standards to matrix matched standards.The effects of different solid phase extraction(SPE)columns were optimized.The use of the SupelMIP SPE Aminoglycoside cartridge kept the analytes bound to the sorbent while a series of aggressive washes were applied to the sorbent to eliminate matrix interferences.The Obelisc R column has reverse phase property and could be applied to conventional reverse phase conditions.It had high density of positive and negative ions on a stationary phase surface,its adsorption capacity in polar compounds could be greatly improved compared with the traditional revers-phase chromatographic column.This allows retaining polar compounds without using ion pairing reagents.The content of acetonitrile and pH of buffer were adjusted so that the9AGs were better retained and separated.T

关 键 词：氨基糖苷类药物 亲水性色谱柱 分子印迹固相萃取 高效液相色谱串联质谱(HPLCMS/MS) 

分 类 号：O657.63[理学—分析化学]