Sørensen Jens Laurids, Nielsen Kristian Fog, Thrane Ulf
Center for Microbial Biotechnology, BioCentrum-DTU, Technical University of Denmark, Building 221, DK-2800 Kgs. Lyngby, Denmark.
J Agric Food Chem. 2007 Nov 28;55(24):9764-8. doi: 10.1021/jf0715875. Epub 2007 Oct 26.
A novel HPLC method was developed for detection of the Fusarium mycotoxin, moniliformin in whole maize plants. The method is based on hydrophilic interaction chromatography (HILIC) on a ZIC zwitterion column combined with diode array detection and negative electrospray mass spectrometry (ESI(-)-MS). Samples were extracted using acetonitrile-water (85:15), and the extracts were cleaned up on strong anion exchange columns. By this procedure we obtained a recovery rate of 57-74% moniliformin with a limit of detection at 48 ng/g and a limit of quantification at 96 ng/g using UV detection at 229 nm, which is comparable to current methods used. Limit of detection and quantification using ESI(-)-MS detection was 1 and 12 ng/g, respectively. Screening of maize samples infected with the moniliformin producing fungi F. avenaceum, F. tricinctum, or F. subglutinans detected moniliformin levels of 1-12 ng/g in 15 of 28 samples using ESI(-)-MS detection. To our knowledge this is the first example of HILIC separation in mycotoxin analysis.
开发了一种新型高效液相色谱法,用于检测全株玉米中的镰刀菌霉菌毒素——串珠镰刀菌素。该方法基于在ZIC两性离子柱上的亲水作用色谱(HILIC),结合二极管阵列检测和负离子电喷雾质谱(ESI(-)-MS)。样品用乙腈-水(85:15)提取,提取物在强阴离子交换柱上净化。通过该程序,使用229 nm紫外检测时,串珠镰刀菌素的回收率为57-74%,检测限为48 ng/g,定量限为96 ng/g,这与目前使用的方法相当。使用ESI(-)-MS检测时,检测限和定量限分别为1和12 ng/g。对感染产生串珠镰刀菌素的真菌燕麦镰刀菌、三线镰刀菌或胶孢镰刀菌的玉米样品进行筛选,使用ESI(-)-MS检测时,在28个样品中的15个中检测到串珠镰刀菌素水平为1-12 ng/g。据我们所知,这是霉菌毒素分析中HILIC分离的首个实例。