摘要
基于表面活性剂能提高荧光强度,分散液相微萃取能提高萃取率,建立测定小麦粉中过氧化苯甲酰的荧光分光光度法。讨论了溶剂种类,优化了测定温度、缓冲溶液、表面活性剂种类和用量对过氧化苯甲酰荧光强度的影响;讨论了萃取剂、分散剂的种类及用量。结果表明:无水乙醇溶液,冰浴,不加缓冲液,加100μL吐温-80(2 g/L),用70μL二氯甲烷做萃取剂和140μL乙腈做分散剂,超声1min对小麦粉样品进行预处理。在1cm微量比色皿中,激发波长(λex)为285nm,于发射波长(λe_m)310nm处读出荧光强度。在0.17~6.00μg/m L范围内,过氧化苯甲酰浓度与其荧光强度线性关系良好,相关系数为0.9993,检出限为0.2028 mg/kg。加标水平在1.29~2.55 mg/kg范围内,回收率为96.9%~105.6%,RSD为5.80%~6.80%(n=3)。新建方法可用于小麦粉中过氧化苯甲酰含量测定。
Based on surfactants can increase fluorescence intensity and dispersive liquid-liquid microextraction can improved the extraction rate,a new fluorimetric method was developed for the determination of Benzoyl peroxide in wheat flour.The kind of solvent,the optimized temperature,buffer solution,the type and the amount of surfactant on the fluorescence intensity of benzoyl peroxide were discussed.The type and dosage of extrcactant and dispersant were also studied.The results showed that anhydrous ethanol was used as solution,water bath,no buffer solution,1 μL tween-80（2 g/L）,70 μL dichloromethane were used as extractant and 140μL acetonitrible was used as dispersant.Ultrasonic extraction time was 1min.The standard and sample solution were added into 1cm trace fluorescence cuvette.Excitation wavelength was 285 nm,fluorescence intensity was read at the emission wavelength of 310 nm.The results showed that in the range of 0.17 ~ 6.00 μg/m L,the concentration of Benzoyl peroxide and the flurescence intensity had a good linearity with the correlation coefficients of 0.9993.The detection limit was 0.2028mg/kg.At spiked levels of 1.29 to 2.55mg/kg,the sample recovery ranges from 96.9% to 105.6%.The relative standard deviation was 5.8% to 6.8%（n=3）.The results demonstrated that the new method proposed in this work could be used for the determination of benzoyl peroxide in wheat flour.
出处
《中国食品添加剂》
北大核心
2017年第4期163-167,共5页
China Food Additives
基金
河北省省级科技计划自筹经费项目(15275511)
河北大学实验室开放项目(sy201670)
“十三五”国家现代农业产业体系(CARS-07-13.5-A16)
关键词
过氧化苯甲酰
分散液相微萃取
荧光分光光度法
吐温-80
小麦粉
benzoyl peroxide
dispersive liquid-liquid microextraction
fluorescence spectrophotometry
Tween-80
wheat flour
