摘要
建立了谷物中脱氧雪腐镰刀菌烯醇DON的高效液相色谱检测和质谱确证方法.样品用水提取,通过免疫亲和柱进行富集和净化,以Hypersil BDS C18柱为分离柱,乙腈-水(10∶ 90,V/V)混合溶剂为流动相进行高效液相色谱分离和检测,利用大气压化学电离质谱(APCI)进行阳性结果的鉴定和确认.在小麦、大麦和面粉等样品中,本方法在0.1~10 μg/g添加范围内的回收率为82.4%~103%,相对标准偏差1.4%~7.6%,检出限0.1 μg/g.
A method was developed for the determination of deoxynivalenol ( DON ) by high performance liquid chromatography (HPLC) and verified by liquid chromatography-mass spectrometry (LC-MS). Samples were extracted and enriched by water, and purified by imunoaffmity columns. DON was quantified by reversed-phase HPLC with Hypersil BDS C18 column and mobile phase of acetonitrile-water (10:90) was used for assay. The positive results were indentified and verified by LC-MS with atmospheric pressure chemical ionization(APCI) source. Recoveries from the different cereals (wheat, barly, flour) spiled with DON at levels ranging from 0.1 to 10 μg/g were from 82.4% to 103%, and relative standard deviations were from 1.4% to 7.6%, the limit of detection was 0. 1 μg/g.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2005年第11期1643-1646,共4页
Chinese Journal of Analytical Chemistry