【摘要】 目的建立高效液相色谱法检测米面及制品中过氧化苯甲酰与富马酸二甲酯的分析方法。方法样品中的过氧化苯甲酰与富马酸二甲酯用50%甲醇水溶液为提取液,超声提取10min,静置3min,加20g/L FeSO4溶液与5%乙酸溶液各0.5 mL,振荡混匀后超声提取10 min, 10000 r/min离心3 min后取上清液过0.22μm水相微孔滤膜待测。对50 mg/L的过氧化苯甲酰与富马酸二甲酯混合标准溶液色谱峰进行光谱扫描,选择220nm作为高通量检测方法的测定波长。采用Agilent ZORBAX Eclipse Plus C18(4.6 mm×150 mm, 5.0μm)色谱柱进行分离,以20mmol/L乙酸铵溶液:甲醇=70:30(V:V)为流动相,外标法定量。结果过氧化苯甲酰与富马酸二甲酯在0～100mg/L范围内,浓度与色谱峰面积的大小分别成正比例线性关系,过氧化苯甲酰线性方程为:Y=23.11X,相关系数为0.999;富马酸二甲酯线性方程为:Y=35.97X,相关系数为0.999。两者的方法检出限为0.40 mg/kg。在0.40、0.80、4.00 mg/kg水平进行加标回收试验与精密度试验,过氧化苯甲酰的回收率分别为85.0%、88.8%、94.0%,相对标准偏差分别为7.9%、6.7%、4.4%;富马酸二甲酯的回收率分别为82.5%、87.5%、94.5%,相对标准偏差分别为7.2%、7.1%、5.4%。结论该方法符合GB/T 27404-2008《实验室质量控制规范食品理化检测》的相应技术要求,方法准确稳定可靠,满足米面及制品中过氧化苯甲酰与富马酸二甲酯的高通量测定。更多还原

【Abstract】 Objective To establish a method for the determination of benzoyl peroxide and dimethyl fumarate in rice, flour and their products by high performance liquid chromatography(HPLC). Methods The benzoyl peroxide and dimethyl fumarate in the sample were extracted with 50% methanol solution, ultrasonically extracted for 10 min,allowed to stand for 3 min, and 20 mL/L of FeSO4 solution and 0.5 mL of 5% acetic acid solution were added. After homogenization and ultrasonic extraction for 10 min, centrifugation at 10000 r/min for 3 min, the supernatant was taken through a 0.22 μm aqueous microporous membrane for testing. The peak of the mixed standard solution of 50 mg/L benzoyl peroxide and dimethyl fumarate was used for spectral scanning, and 220 nm was selected as the measurement wavelength of the high-throughput detection method. The Agilent ZORBAX Eclipse Plus C18(4.6 mm×150 mm,5.0 μm) column was used for separation, and the mobile phase was 20 mmol/L ammonium acetate solution:methanol=70:30(V:V), and quantified by external standard method. Results When benzoyl peroxide and dimethyl fumarate were in the range of 0?100 mg/L, the concentration was proportional to the peak area of the chromatographic peak. The linear equation of benzoyl peroxide was: Y=23.11 X, with the correlation coefficient of0.999, and the linear equation of dimethyl fumarate was: Y=35.97 X, with the correlation coefficient of 0.999. The limits of detection of both analytes were 0.40 mg/kg. At the spiked concentrations of 0.40, 0.80 and 4.00 mg/kg, the recoveries of benzoyl peroxide were 85.0%, 88.8% and 94.0%, respectively, and the relative standard deviations were7.9%, 6.7%, and 4.4%, respectively. The recoveries of dimethyl fumarate were 82.5%, 87.5% and 94.5%,respectively, and the relative standard deviations were 7.2%, 7.1% and 5.4%, respectively. Conclusion This method meets the corresponding technical requirements of GB/T 27404-2008 Laboratory quality control specification food physical and chemical testing, and the method is accurate, stable and reliable, which meets the high-throughput determination of benzoyl peroxide and dimethyl fumarate in rice, flour and their products.更多还原