腐乳中桔霉素提取条件优化及检测方法研究

Study on method of detection and optiminzation of extracted conditions for citrinin in sufu

对腐乳中桔霉素提取条件进行优化,确定最佳提取条件为甲苯—乙酸乙酯—甲酸（7∶3∶1,V/V）超声处理10min,提取温度50℃,提取3次,提取液经浓缩后甲醇定容。建立高效液相色谱荧光检测器法测定腐乳中桔霉素,采用Hypersil ODS 2（250 mm×4.6 mm,5μm）为分析柱,水（p H2.5）—乙腈（70∶30,V/V）为流动相,流速0.8 m L/min,采用荧光检测器分析,外标法定量。结果表明：桔霉素在0.01-100.00μg/m L范围内线性良好（R2=0.999 99）,检出限0.005 mg/kg,样品加标回收率为90.4%-107.9%,相对标准偏差（RSD6）小于6%,该方法操作简便、结果可靠。

Extracted conditions for citrinin were optimized in sufu.Citrinin was extracted completely by toluene-ethyl acetate-formic acid（7 ∶ 3 ∶ 1,V / V） at 50 ℃,with 10 min ultrasonic processing.A method for determining citrinin in sufu was established by high performance liquid chromatography（HPLC） with fluorescence detection.Citrinin was separated by mobile phase of water（p H 2.5）-acetonitrile（70∶ 30） on Hypersil ODS2 column.The results were showed that there was good linear relationship between the fluorescence detection values and citrinin concentration in the range of 0.01 - 100.00 μg / m L（R2= 0.999 99）.The limit of detection was 0.005 mg / kg and the recovery of citrinin were between 90.4% and107.9% and relative standard deviation（RSD,n = 6） value were less than 6%.