免疫亲和柱净化-高效液相色谱法测定大米、玉米、辣椒中的橘霉素

建立免疫亲和柱净化-高效液相色谱法测定农产品中橘霉素的方法。试样经甲醇-水提取，稀释、过滤后通过含有橘霉素特异性抗体的免疫亲和柱净化，洗脱液用C18色谱柱、乙腈-三氟乙酸溶液(60:40，V/V)分离，荧光检测器测定(激发波长331nm，发射波长500nm)，外标法定量。结果表明：色谱峰面积与橘霉素含量之间有良好的线性关系，方法的检出限为10μg/kg，定量限为30μg/kg，加标回收率为61%～96.6%，相对标准偏差为3.72%～6.40%。该方法操作简便、准确，回收率高、精密度良好、重现性好，可用于大米、玉米、辣椒中橘霉素的测定。

Determination of Citrinin in Agricultural Products by Immunoaffinity Column Clean-up Coupled with HPLC

A HPLC coupled with immunoaffinity column cleanup method for the determination of citrinin in agricultural products such as rice, corn and pepper was established. Samples were extracted with methanol aqueous solution and cleaned up on a column containing anti-citrinin specific antibody. The chromatographic separation was performed on a C18 column (150 mm × 4.6 mm, 5μm) eluted by a mobile phase composed of acetonitrile and TFA solution at a ratio of 60:40 (V/V). A fluorescence detector with 331 nm excitation wavelength and 500 nm emission wavelength was used for the quantification of citrinin in an external standard mode. Peak area and citrinin concentration displayed an excellent linear relationship. The limit of detection of this method was 10μg/kg and limit of quantitation was 30μg/kg. The spike recovery rates for citrinin were between 61% and 96.6%, with relative standard deviations ranging from 3.72% to 6.40%. This method has the characteristics of ease of operation, accuracy, high recovery, excellent precision and good reproducibility and is suitable for the determination of citrinin in rice, corn and pepper.