液质联用同位素内标法同时测定3类小麦终产品中4种B类单端孢烯霉族类真菌毒素  

Detection of 4 kinds of type B trichothecene mycotoxins in wheat end products using high performance liquid chromatography-mass spectrometry with isotope internal standard

作　　者：朱芸[1] 雒婉霞[1] 赵清荣[1] 杨雪丽[1] 王冉冉[1] 王猛[1] 

机构地区：[1]新疆维吾尔自治区疾病预防控制中心,新疆乌鲁木齐830002

出　　处：《中国卫生检验杂志》2017年第13期1863-1866,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立测定小麦终产品中4种B类单端孢烯霉族类真菌毒素的液质联用同位素内标法。方法馍馍、面包、面条3类样品粉碎混匀后经乙腈-水溶液(84∶16,V/V)提取,Romer Myco Sep 226多功能净化柱净化,Thermo TSQ Quantum Access Max三重四级杆质谱电喷雾负离子源(ESI-),多反应监测(MRM)方式进行检测,同位素内标法定量。结果 4种真菌毒素在5.00μg/L^500μg/L呈良好线性关系(r≥0.999 0),检出限为0.18μg/kg^0.25μg/kg,精密度相对标准偏差为2.46%~10.30%,加标回收率为70.8%~107.6%。结论此方法灵敏度高,线性范围较宽,可满足不同浓度的小麦终产品中4种真菌毒素的同时检测。Objective To establish a method for the simultaneous determination of 4 kinds of type B trichothecene mycotoxins in wheat end products using high performance liquid chromatography-mass spectrometry（ LC-MS/MS）. Methods Three kinds of wheat flour products including steamed bun,bread and noodles were crushed and extracted with acetonitrile-water（ 84∶16,V/V）,then purified with Romer Myco Sep 226 column. The trichothecene mycotoxins were detected by UPLC-MS/MS system using negative electrospray ionization（ ESI-） in multiple-reaction monitoring（ MRM） mode,and quantified by the internal standard calibration curve of isotope dilution technique. Results 4 kinds of mycotoxins showed good linearity in the range of5. 00 μg/L-500 μg/L,with the correlation coefficients（ r） ≥0. 999 0,the LODs of the mycotoxins ranged from 0. 18 μg/kg to0. 25 μg/kg. Meanwhile,the precision was within 2. 46%-10. 30%,and the average recovery was within 70. 8%-107. 6%.Conclusion The method was suitable for detecting 4 kinds of mycotoxins simultaneously in wheat end products at different concentrations with high accuracy,sensitivity and wide linear range.

关 键 词：同位素内标 液质联用 小麦终产物 真菌毒素 

分 类 号：O657.63[理学—分析化学]