超高效液相色谱-串联质谱法检测毛发中的玉米赤霉烯酮

Detection of Zearalenone by UPLC-MS/MS in Hair

目的基于超高效液相色谱-串联质谱技术,建立毛发中玉米赤霉烯酮的分析方法,为玉米赤霉烯酮的检测提供简捷、高效、可靠的分析测定方法。方法毛发样品经冷冻研磨后加入0.5 m L乙腈,置于冰水浴中超声30 min,采用AcquityTMUPLC HSS T3色谱柱分离,电喷雾负离子源进行离子化,多反应监测方式（MRM）对玉米赤霉烯酮的母离子及子离子进行监测,三重四极杆质谱测定。结果该方法在5～250 pg/mg范围线性良好：Y=0.007x＋0.044（R2=0.999）;玉米赤霉烯酮的检出限为2 pg/mg,定量限为5 pg/mg;提取回收率为90.9%～95.3%;基质效应88.2%～92.5%;准确度为93.5～107.8%,日内及日间精密度（RSD）均小于10%。结论本方法简便快速、灵敏度高、专属性强,可满足在食品安全和司法鉴定实践中对毛发中玉米赤霉烯酮测定的要求。

Objective To establish a sensitive and reproducible method for the quantitative analysis of zearalenone（ZON） in hair samples by UPLC-MS/MS. Method The hair samples were prepared using a frozen pulverization preparation method. 0.5m L of acetonitrile was added to 20 mg of hair powder, in the presence of Estriol used as internal standard, then the sample was sonicated for 30 minutes in ice bath. After high-speed centrifugation, the supernatant was analyzed by UPLC-MS/MS. The UPLC separation was performed on an AcquityTMUPLC HSS T3 column with a linear gradient elution program of 0.1%（v/v）formic acid solution and acetonitrile as the mobile phase. Multiple reaction monitoring（MRM） was used for the selective detection of ZON. Results The linearity curve of ZON in the range from 5 to 250 pg/mg was Y=0.007x＋0.044（R2=0.999）. And the limit of quantification was 5pg/mg in spiked hair samples. The recoveries of ZON were 90.9% ~95.3%, the inter-day and intra-day relative standard deviations（RSD） were less than 10%. Conclusion The established method is simple, rapid, sensitive and specific, and is appropriate for the identification and quantification of ZON in human hair.