Rice L G, Ross P F, Dejong J, Plattner R D, Coats J R
U.S. Department of Agriculture, National Veterinary Services Laboratories, Ames, IA 50010, USA.
J AOAC Int. 1995 Jul-Aug;78(4):1002-9.
The performance of a liquid chromatographic method for determining fumonisins in corn, animal feeds, and culture material was evaluated. Efficiencies of extractions with the following solvent systems were determined: acetonitrile-water (50 + 50, v/v), methanol-water (75 + 25, v/v), and 100% water. The acetonitrile solvent gave both higher extraction efficiencies and faster extraction times than the other 2 solvents. Extraction was followed by C18 solid-phase extraction column cleanup. Fumonisin B1 (FB1), fumonisin B2 (FB2), and fumonisin B3 (FB3) were measured by precolumn derivatization with o-phthalaldehyde followed by isocratic separation on a C18 reversed-phase column with a mobile phase of 50 mM potassium dihydrogen phosphate (pH 3.3)-acetonitrile (60 + 40). Commercially prepared poultry feed, corn, and Fusarium spp. corn cultures were analyzed at the following levels: FB1, 1.5 to 15,000 micrograms/g; FB2, 0.5 to 4000 micrograms/g; FB3, and 0.17 to 1,500 micrograms/g. Recoveries were 91-94%, 90-100%, and 81-93% for FB1, FB2, and FB3, respectively. Precision (coefficient of variation) was determined with pooled field samples and ranged from 2% at 19 micrograms/g for FB1 to 9% at 0.17 microgram/g for FB3. Time and pH studies of the formation of the fluorescent derivative and its stability were conducted. Complete reaction occurred at pHs above 7.9, with optimal pH for chromatography between 8.0 and 8.5. No statistically significant response differences were detected for reaction times ranging from 4 to 40 min; however, the detector signal was significantly reduced when reaction times were shorter than 4 min. Chromatograms of samples were free of interferences for all feeds, corn, and culture material tested.(ABSTRACT TRUNCATED AT 250 WORDS)
对一种用于测定玉米、动物饲料和培养材料中伏马菌素的液相色谱方法的性能进行了评估。测定了以下溶剂体系的萃取效率：乙腈 - 水（50 + 50，v/v）、甲醇 - 水（75 + 25，v/v）和100%水。与其他两种溶剂相比，乙腈溶剂具有更高的萃取效率和更快的萃取时间。萃取后用C18固相萃取柱进行净化。伏马菌素B1（FB1）、伏马菌素B2（FB2）和伏马菌素B3（FB3）通过邻苯二甲醛柱前衍生化，然后在C18反相柱上进行等度分离，流动相为50 mM磷酸二氢钾（pH 3.3） - 乙腈（60 + 40）来测定。对市售家禽饲料、玉米和镰刀菌属玉米培养物进行了如下水平的分析：FB1，1.5至15,000微克/克；FB2，0.5至4000微克/克；FB3，0.17至1500微克/克。FB1、FB2和FB3的回收率分别为91 - 94%、90 - 100%和81 - 93%。用混合田间样品测定精密度（变异系数），范围从FB1在19微克/克时的2%到FB3在0.17微克/克时的9%。进行了荧光衍生物形成及其稳定性的时间和pH研究。在pH高于7.9时发生完全反应，色谱分析的最佳pH为8.0至8.5。对于4至40分钟的反应时间，未检测到统计学上显著的响应差异；然而，当反应时间短于4分钟时，检测器信号显著降低。所测试的所有饲料、玉米和培养材料的样品色谱图均无干扰。（摘要截短为250字）
