固相萃取-液相色谱-质谱/质谱法同时测定蜂蜜中的多类药物残留

摘要

A method of solid pnase extraction-liquid cnromatograpny-tanaem mass spectrome-try (SPE-LC-MS/MS) for simultaneous determination of 54 drug residues (sulfonamides, nitro-imidazoles, quinolones, macrolides, lincosamides and praziquantel) in honey was developed. The honey samples were diluted by phosphate buffer solution (Ph 8) followed by a further cleanup procedure with an Oasis (HLB) SPE column. The detection was carried out by LC-MS/ MS, using positive-ion electrospray ionization in multiple reaction monitoring (MRM) mode, with one precursor/two product ion transitions for each compound. Isotope dilution internal standard method or external standard method was used to determine the residue contents with a good linear relationship (r > 0. 992). The limits of quantification (LOQs, S/N > 10) were 1. 0 μg/kg for sulfonamides and nitroimidazoles, 2.0 μg/kg for quinolones and lincosamides, 3.0 μg/kg for macrolides, and 0. 3 μg/kg for praziquantel. The recovery ranges were from 32. 6% to 114% with the relative standard deviations (RSDs) between 1. 3% and 28. 9%. As a screening method, the developed procedure is suitable for the determination and confirmation of the drug residues in honey samples.%建立了采用固相萃取-液相色谱-质谱/质谱(SPE-LC-MS/MS)对蜂蜜中磺胺类、硝基咪唑类、喹诺酮类、大环内酯类、林可酰胺类和吡喹酮共计6大类54种药物残留同时测定的方法.蜂蜜经磷酸盐缓冲溶液(pH 8)稀释,Oasis HLB固相萃取柱净化后,通过液相色谱-质谱联用技术进行检测(正离子方式,多反应监测模式).采用同位素稀释内标法或外标法进行定量,线性关系良好,相关系数大于0.992.方法的定量限(LOQ,以信噪比(S/N)大于10计)分别为磺胺类和硝基咪唑类药物1.0μg/kg,喹诺酮类和林可酰胺类药物2.0μg/kg,大环内酯类药物3.0μg/kg,吡喹酮0.3μg/kg.总体回收率为32.6％～114％,相对标准偏差为1.3％～28.9％.该方法的定量限满足目前国内外药物的最大残留限量要求,可作为蜂蜜中相关约物残留量的筛选检测方法.