超高效液相色谱-串联质谱法测定谷物中的杂色曲霉素  

Determination of sterigmatocystin in different grains by ultra-performance liquid chromatography tandem mass spectrometry

作　　者：刘少颖[1] 黄希汇[1] 樊继彩[1] 金铨[1] 

机构地区：[1]杭州市疾病预防控制中心,浙江杭州310021

出　　处：《中国卫生检验杂志》2016年第16期2281-2284,共4页Chinese Journal of Health Laboratory Technology

基　　金：浙江省医药卫生科技计划项目(2014KYA188)

摘　　要：目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)测定玉米、大米、小麦等谷物食品中潜在的致癌物——杂色曲霉素的方法。方法通过优化液相色谱与质谱的采集参数,得到适用于杂色曲霉素的最佳仪器检测条件。谷物样品经改良的Qu ECh ERS前处理技术进行提取净化。通过优化提取溶液和净化吸附剂,最终确定前处理步骤为谷物样品加水浸泡后再用乙腈提取,经C_(18)吸附剂净化,有效降低了样品基质带来的背景干扰,最终在UPLC-MS/MS的多反应监测模式(MRM)下进行内标法定量。结果杂色曲霉素在0.1 ng/ml^10.0 ng/ml时,线性关系良好,检出限(LOD)和定量限(LOQ)分别为0.09μg/kg^0.16μg/kg和0.30μg/kg^0.53μg/kg;在低、中、高3种浓度(1.0μg/kg、5.0μg/kg、10.0μg/kg)添加水平下,回收率为80.3%~102.1%,相对标准偏差(RSD)为3.61%~15.04%。结论该方法简便、灵敏、准确、稳定,适用于谷物中杂色曲霉素的测定。Objective To establish a method for the determination of the potential carcinogen,sterigmatocystin in different grains by ultra-performance liquid chromatography tandem mass spectrometry（UPLC-MS）.Methods Through the optimization of liquid phase chromatography and mass spectrometry acquisition parameters,the best instrument detection conditions for the detection of sterigmatocystin were obtained.The samples were extracted and purified using a modified Qu ECh ERS method.By optimizing the extraction solution and purification adsorbent,the pre-processing steps for cereal samples was extraction with acetonitrile after soaking with water,and the sample was then purified by C（18） with adsorbent,which effectively reduced the background interference caused by sample matrix;and finally quantified with internal standard method in multiple reaction monitoring mode（MRM）.Results Good linearity was obtained when the concentration of sterigmatocystin was within 0.1 ng/mL-10.0 ng/mL.The limits of detection（LODs） and limits of quantification（LOQs） were within 0.09 μg/kg-0.16 μg/kg and0.30 μg/kg-0.53 μg/kg,respectively.Satisfactory recoveries（80.3%-102.1%） of sterigmatocystin in different grains were demonstrated at different spiked levels（1.0 μg/kg,5.0 μg/kg,10.0 μg/kg）,and the relative standard deviations（RSDs）were among 3.61%-15.04%.Conclusion The method was simple,sensitive and accurate,which is suitable for the detection of sterigmatocystin in grains.

关 键 词：超高效液相色谱-串联质谱 谷物 杂色曲霉素 

分 类 号：O657.63[理学—分析化学]