多功能净化柱-超高效液相色谱-串联质谱法测定挂面、方便面中4种真菌毒素  

Determination of 4 kinds of mycotoxins in dried noodles and instant noodles by multifunctional columns-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：孙卫明[1] 王权帅[1] SUN Wei-Ming;WANG Quan-Shuai(Huairou District Center for Disease Control and Prevention,Beijing 101400,China)

机构地区：[1]北京市怀柔区疾病预防控制中心,北京101400

出　　处：《中国卫生检验杂志》2021年第6期662-665,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立多功能净化柱-超高效液相色谱-串联质谱法测定挂面、方便面中玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇及其衍生物等4种真菌毒素含量。方法用乙腈-水-甲酸(84∶15∶1,体积比)溶液进行提取,采用226多功能净化柱净化,内标法定量。对超高效液相色谱-串联质谱仪的仪器测定条件,分别进行优化和摸索,最后对建立的方法进行方法学实验。结果该方法对玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇及其衍生物等4种真菌毒素有很好的分离效果,检出限为3.0μg/kg~6.0μg/kg,回收率在80.2%~110.6%,精密度在2.1%~7.9%,相关系数≥0.999 0。结论本方法操作简便、快速,灵敏度、精密度、回收率均满足方法学要求,适用于挂面、方便面中玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇及其衍生物等4种真菌毒素含量的同时测定。Objective To establish a method for the determination of 4 kinds of mycotoxins in dried noodles and instant noodles by multifunctional columns-ultra high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile-water-formic acid( 84∶15∶1,V∶V∶V) solutions,cleaned-up by 226-multifunctional columns,isotope internal standards were used for quantification. The instrument conditions of the ultra high performance liquid chromatography-triple quadrupole mass spectrometer were optimized and explored. Finally,methodological experiments were carried out to satisfy the test requirements. Results The separation of 4 kinds of mycotoxins was very well. The limit of detection( l OD) was within 3. 0 μg/kg-6. 0 μg/kg,and the recoveries were within 80. 2%-110. 6%. The precision range was within 2. 1%-7. 9% and the correlation coefficients were ≥0. 999 0. Conclusion This method is simple and rapid,the sensitivity,precision and recovery are all satisfied with the methodological requirements,which can be suitable for the simultaneous determination of 4 kinds of mycotoxins in dried noodles and instant noodles.

关 键 词：真菌毒素 超高效液相色谱-串联质谱法 多功能净化柱 挂面 方便面 

分 类 号：O657.63[理学—分析化学]