蜂蜜中硝基呋喃代谢物的超高效液相色谱-串联质谱测定法  

Determination of nitrofuran metabolites in honey by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：高洋洋[1] 刘鑫 陈广全 GAO Yang-yan;LIU Xin;CHEN Guang-quan(Physical and Chemical Inspection,Xicheng District Center for Disease Control and Prevention,Beijing, 100120,China;Food Laboratory,Inspection and Quarantine Technology Center,Beijing Entry Exit Inspection and Quarantine Bureau,Beijing, 100026,China)

机构地区：[1]北京市西城区疾病预防控制中心理化检验科,北京100120 [2]北京出入境检验检疫局检验检疫技术中心食品实验室,北京100026

出　　处：《职业与健康》2018年第13期1764-1768,共5页Occupation and Health

基　　金：省部级北京市科技重大专项首都食品质量安全保障(Z171100001317011)

摘　　要：目的采用超高效液相色谱-串联质谱法(UPLC-MS/MS)测定蜂蜜中的呋喃它酮(AMOZ)、呋喃西林(SEM)、呋喃妥因(AHD)和呋喃唑酮(AOZ)等4种硝基呋喃代谢物的分析方法。方法试样经2-硝基苯甲醛衍生化,调节pH值至7.0~7.5,衍生溶液用Oasis HLB固相萃取柱净化,乙酸乙酯洗脱,流动相定容,采用选择反应监测(SRM)模式检测,同位素内标法定量。结果硝基呋喃代谢物在0.5~30.0μg/L范围内线性关系良好(r>0.997)。方法的检出限为0.5μg/kg,在0.5、1.0、2.0μg/kg的添加浓度的回收率为83.5%~101.9%,相对标准偏差(RSD,n=6)在3.21%~5.46%之间。结论该方法快速、灵敏和准确,适合蜂蜜中硝基呋喃代谢物的测定。[Objective]To establish a method for determination of nitrofuran metabolites[furaltadone（AMOZ）,furazolidin（SEM）,furantoin（AHD）,and furazolidone（AOZ）] in honey by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.[Methods]Samples were derivatized with 2-nitrobenzaldehyde and adjusted the pH 7.0 to 7.5. The derivatized solutions were cleaned up by Oasis HLB solid extraction column nd the target compounds were eluted with ethylacetate.The analysis were carried out in the selective reaction monitoring（SRM） mode and internal standard isotope dilution method was used for quantification.[Results] The calibration curve showed a good linearity in the range of 0.5-30.0 μg/l and the correlation coefficient（r） was higher than 0.997. The detection limit was 0.5 μg/kg. At the spiked levels of 0.5,1.0 and 2.0 μg/kg,the recoveries of trimethoprim ranged from 83.5 % to 101.9 % and the relative standard deviation（RSD,n=6） ranged from 3.21 % to5.46 %.[Conclusion]The method is simple,rapid,sensitive and suitable for the determination of nitrofuran metabolites in honey.

关 键 词：硝基呋喃代谢物 蜂蜜 超高效液相色谱串联-质谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]