title: [Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].
abstract: 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 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, 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 cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.
authors: Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China. huang-juan@yeah.net
authors: Juan
authors: J
authors: Huang
authors: Guosong
authors: G
authors: Chen
authors: Xiaoyan
authors: X
authors: Zhang
authors: Chongyu
authors: C
authors: Shen
authors: Chen
authors: C
authors: Lü
authors: Bin
authors: B
authors: Wu
authors: Yan
authors: Y
authors: Liu
authors: Huilan
authors: H
authors: Chen
authors: Tao
authors: T
authors: Ding
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D018556:Crops, Agricultural / Q000737:chemistry*; D002523:Edible Grain / Q000737:chemistry; D005504:Food Analysis / Q000379:methods; D005506:Food Contamination / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014255:Trichothecenes / Q000032:analysis*; D014908:Triticum / Q000737:chemistry; D003313:Zea mays / Q000737:chemistry
chemical_list: D014255:Trichothecenes; C007262:deoxynivalenol