UPLC–Q–Orbitrap HRMS 结合全碳标记稳定同位素内标法精确测定粮油中黄曲霉毒素

建立了全自动免疫亲和柱净化–超高效液相色谱–四级杆/静电场轨道阱高分辨质谱（UPLC-Q-Orbitrap HRMS）结合全碳标记稳定同位素内标法对粮油中四种黄曲霉毒素精确定量方法。样品准确称量后加入全碳标记稳定同位素内标，经84/16(V/V)的乙腈/水提取、离心、稀释后，通过全自动固相萃取仪采用黄曲霉毒素免疫亲和柱进行全自动净化，净化液在UPLC-Q-Orbitrap HRMS上进行检测后采用内标法进行定量分析。结果表明：黄曲霉毒素的加标回收率为84.7%～104.6%，日内相对标准偏差为1.7%～9.4%，日间精密度为0.7%～8.4%。采用本方法对国家标准物质的检测结果在赋值范围内，能够最大限度地降低实验人员工作量，提高工作效率，避免因人员操作失误导致的结果偏差，适用于粮油中黄曲霉毒素的精准测定，可满足日常检测和监测需求。

Accurate Determination of Aflatoxin in Grains and Oils use Liquid Chromatography Mass Spectrometry Purified by Automatic Solid Phase Extraction Instrument and Quantified by Fully 13C-Labelled Internal Standards

An UPLC Quadrupole Orbitrap high resolution mass Spectrometry method for accurate quantification of aflatoxins in grains and oils was established, which were purified by automatic immunoaffinity column. The sample was extracted with 84/16(V/V) acetonitrile/water and centrifuged. The supernatant was diluted 10 times with 0.1% PBST. Aflatoxin immunoaffinity column without background and recovery greater than 90% was chosen for purification automatically. UPLC-Quadrupole Orbitrap HRMS was used for quantitative analysis. Results showed that recoveries for aflatoxins were 84.7%~104.6%. The intra-day relative standard deviations were 1.7%~9.4%, and the intra-day precision were 0.7%~8.4%. The developed method can minimize the workload, improve work efficiency and avoid the result deviation caused by operation manually. It is suitable for the accurate determination of aflatoxins in grains and oils, and meet the requirement of the daily test and monitoring aflatoxins.