杂色曲菌素HPLC检测方法的建立及其在大米污染样品中的运用

HPLC Determination of Versicolorin A in Aspergillus parasiticus Contaminated Rice

采用自制杂色曲菌素(VA)标准品,建立大米中杂色曲菌素的高效液相色谱检测方法。大米污染样品经丙酮提取、柱色谱净化,HPLC-紫外检测器进行测定,检测波长288nm。结果表明,VA在100～1250ng/mL质量浓度范围内线性关系良好,r>0.999,方法回收率在84.12%～105.12%之间,平均变异系数小于7.5%,最低检测限为50ng/mL。该方法灵敏度较高、稳定性好、成本较低,可以用于粮食中杂色曲菌素的定量检测。

A HPLC method was established for the determination of versicolorin A （VA） in Aspergillus parasiticus contaminated rice using the VA prepared in our laboratory as a reference standard, which was prepared from the fermented mycelia of Aspergillus parasiticus ATCC 36537 through organic solvent extraction followed by semi-preparative HPLC purification. Samples （like rice artificially contaminated with Aspergillus parasiticus GIM 3395 in this study） were extracted with acetone, cleaned up on a silica column and analyzed using a HPLC system equipped with a UV detector at 288 nm wavelength. Results showed that the standard curve of VA exhibited good linearity over the concentration range of 100 to 1250 ng/mL with more than 0.999 correlation coefficient. Average recoveries of 3 replicates of VA in a blank rice sample spiked at 3 levels were between 84.12% and 105.12% with an average relative standard deviation of less than 7.5%. The limit of detection was 50 ng/mL. This method proved to be sensitive, stable and economical and thus is most suitable for the quantification of VA in cereal grains.