测定玉米中伏马毒素的免疫亲和层析净化高效液相色谱法

伏马毒素(Fumonisins)是串珠镰刀菌繁殖产生的一类真菌毒素。玉米在生长和储存过程中极易受到伏马毒素的侵染。流行病学研究结果表明，受到伏马毒素污染的玉米及其制品可导致马白脑软化症、猪肺水肿综合症，还可诱发人类食管癌和胎儿神经管畸形等疾病。本研究建立了应用免疫亲和柱净化高效液相色谱测定玉米中伏马毒素B₁和B₂的方法，同时，运用统计学方法对该法进行了准确性和再现性评价。结果表明，FB₁和FB₂线性范围分别为0.06~5.00 μg mL^-1和0.04~2.50 μg mL^-1，回收率分别为76.6%~93.8%和77.9%~93.4%，FB₁和FB₂方法定量限分别为0.09 mg kg^-1、0.06 mg kg^-1，实验室内重复性测定的变异系数均低于5%，实验室间再现性测定的变异系数低于6%。上述结果说明该方法的线性、准确度、精密度、灵敏度及同一实验室重复性和多家实验室的再现性评价结果优良，适合作为伏马毒素的测定方法。应用该方法对310份玉米进行了伏马毒素的测定，结果表明，大田、存储玉米伏马毒素总量范围分别为0.20~9.06 mg kg^-1、0.21~6.10 mg kg^-1，建议应加强玉米中伏马毒素污染水平监控，保证人畜健康。

Determining Fumonisins in Corn by High Performance Liquid Chromatography with Immunoaffinity Column Cleanup

Fumonisins are mycotoxins produced mainly by Fusarium verticillioides. Corn is frequently found being contaminated by fumonisins during its growth and storage. Epidemic study demonstrated that corn and corn-based products contaminated by fumonisins can cause equine leukoencephalomalacia and swine pulmonary oedema, also induce oesophageal cancer and neural tube defects of mankind. In this paper, a high performance liquid chromatography (HPLC) method with immunoaffinity columncleanup was established to determine the fumonisins B₁ (FB₁) and B₂ (FB₂) in corn. Meanwhile, the accuracy and reproducibility of the method were evaluated by statistical technique. The results showed that the linear ranges of FB₁ andFB₂ were 0.06–5.00 μg mL^-1 and 0.04–2.50 μg mL^-1, the recovery ranges were 76.6–93.8% and 77.9–93.4%, respectively. Thequantification limit of FB₁ andFB₂ was 0.09 mg kg^-1 and 0.06 mg kg^-1, respectively. The coefficient of variation within-laboratory repeatability was below 5%, and that between-laboratories reproducibility was below 6%. Research results indicated that this method possessed good linearity, accuracy, precision, sensitivity, repeatability within a laboratory and among laboratories. Therefore, this method was proved to be suitable for determination of fumonisins in corn. Applying this method, fumonisins in 310 specimens of corn were determined. Results showed that total fumonisins (B₁+ B₂) ranged from 0.20 to 9.06 mg kg^-1 for field corn, and from 0.21 to 6.10 mg kg^-1 for stored corn. It is proposed that monitoring fumonisins’ level in corn should be reinforced to protect the health of man and livestock.