高效液相色谱法同时测定糕点中富马酸二甲酯与纳他霉素

Simultaneous determination of dimethy fumarate and natamycin in cake by HPLC

建立高效液相色谱法同时测定糕点中富马酸二甲酯与纳他霉素的检测方法。样品经10 m L甲醇溶解、超声提取后,采用Phenomenex Gemini C18色谱柱(150 mm×4.6 mm,5μm)分离,以甲醇与20 mmol/L乙酸铵溶液(50∶50,V/V)为流动相,两者分离效果较好。富马酸二甲酯与纳他霉素在0.5~20.0μg/m L质量浓度范围内线性关系良好(R^2=0.999 9),检出限(LOD)(S/N=3)分别为0.04 mg/kg与0.20 mg/kg。加标回收率分别为94.430%~99.616%和95.860%~101.968%,精密度试验结果变异系数(CV)分别为1.09%~2.02%和1.54%~2.66%。该方法与国标方法测定样品中富马酸二甲酯与纳他霉素含量的相对标准偏差(RSD)分别为0.789%和0.918%,符合方法学要求,表明该方法准确可靠、精密度良好,可用于实际样品中富马酸二甲酯与纳他霉素的同时测定。

The detection method was established for the simultaneous determination of dimethy fumarate and natamycin in food by HPLC. After dissolved in 10 ml methanol and extracted with ultrasonic, the sample was separated by Phenomenex Gemini C,8 chromatographic column （150 min× 4.6 mm, 5 μm）. With methanol and 20 mmol/L ammonium acetate solution （50：50, V/V） as mobile phase, the separation efficiency of dimethy fumarate and natamycin was good. The dimethy fumarate and natamycin had a good linear relationship in the range of 0.5-20.0 μg/ml （R2= 0.999 9）, and the limit of detection （S/N=3） were 0.04 mg/kg and 0.20 mg/kg, respectively. The coefficient of variation of precision tests results were 1.09%- 2.02% and 1.54%-2.66%, respectively. The relative standard deviation （RSD） of the method and national standard method for determining the content of dimethy fumarate and natamycin in sample was 0.789% and 0.918%, respectively, which was accorded with the requirements of the methodology. Due to its reliable accuracy and good precision, the method was suitable for simultaneous determination of dimethy fumarate and natamycin in actual sample.