固相萃取-高效液相色谱-串联质谱法检测粮食及其制品中的呕吐毒素

摘要

A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2. 6 (j.m) with a gradient elution using 0. 3%o ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ioni-zation mode. The limit of detection (LOD, S/N = 3) and the limit of quantification (LOQ, S/N = 10) were 20 |xg/kg and 50 |xg/kg, respectively. A good linearity (r >0. 99) was achieved for the target compound over the range of 20 - 1 000 p,g/L. The recoveries at the three spiked levels (50, 100, 500 |j,g/kg) in the blank matrices such as flour, barley, soybean, rice, corn-meal, cassava and wheat, were varied from 75. 6% to 111. 0% with the relative standard deviations no more than 13.0%. The method is accurate, efficient, sensitive and practical. The costof pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.%建立了粮食及其制品中呕吐毒素的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法.样品经乙腈-水(84:16,v/v)溶液提取,HLB固相萃取柱富集净化,采用HPLC-MS/MS法对目标物进行定性确证和定量分析.在Phenomenex Kinetex C18柱(100 mm ×4.6 mm,2.6 μm)上以0.3‰氨水和乙腈为流动相进行梯度洗脱分离；质谱模式为电喷雾负离子监测模式.本方法的检出限(以信噪比(S/N) =3计)和定量限(以S/N=10计)分别为20μg/kg和50 μg/kg;在20 ～1000 μg/L范围内呈现良好的线性关系,相关系数(r)大于0.99.对本底空白的面粉、大麦、大豆、大米、玉米粉、木薯干、小麦等7种代表性基质进行50、100、500 μg/kg 3个含量水平的添加试验,回收率范围为75.6％～111.0％,精密度(以相对标准偏差(RSD)计)不大于13.0％.本方法准确可靠,灵敏度高,经济实用,可替代较为昂贵的免疫亲和柱和多功能净化柱,较大地降低检测成本.