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作 者:陈桐[1,2,3] 鞠昭函 李疆[2] 赵珊[2] 丁晓静[2,3]
机构地区:[1]首都医科大学附属北京安贞医院,北京100029 [2]北京市疾病预防控制中心,北京100013 [3]首都医科大学公共卫生学院,北京100069 [4]北京联合大学应用文理学院,北京100083
出 处:《中国食品卫生杂志》2016年第1期65-69,共5页Chinese Journal of Food Hygiene
基 金:北京市卫生系统高层次卫生技术人才培养项目(2013-2-036)
摘 要:目的建立利用毛细管区带电泳-间接紫外法测定食品中三氯蔗糖的方法。方法样品用超纯水提取,离心所得的上清液直接进样,以未涂层熔融石英毛细管(50μm×60.2 cm)为分离柱,3 mmol/L 3,5-二硝基苯甲酸+10 mmol/L磷酸钠+12 mmol/L氢氧化钠(pH=12.58)+0.5 mmol/L十六烷基三甲基溴化铵为分离缓冲液;检测波长200 nm,分离电压-20 kV。采用校正峰面积外标法进行定量。结果方法检出限为10 mg/L,定量限为30 mg/L,线性范围为30-300 mg/L,线性相关系数r=0.9991。低、中、高3个质量浓度(40、60及80 mg/L)的加标回收率分别为108.1%、102.6%、103.5%,相对标准偏差(RSD)分别为1.3%、1.3%及1.0%,方法精密度为2.0%。结论本研究样品前处理操作简单,20 min之内即可完成三氯蔗糖的含量分析(预清洗6 min,分离13 min),实现了与其结构相似但又同时存在于食品中蔗糖的分离,且试剂及样品消耗量少,适用于实验室对于食品中三氯蔗糖的检测。Objective To develop a new method for the determination of sucralose in foods by capillary zone electrophoresis with indirect ultraviolet detection. Methods Samples were extracted with ultrapure water and then centrifuged. The separation was carried out using an uncoated fused-silica capillary. The separation buffer consisted of3 mmol / L 3,5-dinitrobenzoic acid,10 mmol / L sodium phosphate,12 mmol / L sodium hydroxide( pH = 12. 58) and0. 5 mmol / L hexadecyltrimethylammonium bromide. The separation voltage was- 20 k V and the detection wavelength was200 nm. Quantification was made by external calibration between the corrected peak areas and the concentrations of sucralose. Results The limit of detection and limit of quantitation were 10 and 30 mg / L,respectively. The linear range between the corrected peak area and the concentration was from 30 to 300 mg / L with a correlation coefficient of 0. 999 1.The average spiked recoveries of five replicates at three levels( 40,60 and 80 mg / L) were 108. 1%,102. 6% and103. 5% with relative standard deviations of 1. 3%,1. 3% and 1. 0%,respectively. The precision of the method was2. 0%. Conclusion The method is simple with minimal sample and reagent consumption. The analysis could be completed within 20 min( 6 min for rinsing and 14 min for separation). Sucralose could be baseline separated from sucrose with similar structure. Five kinds of food samples( a total of eight) were analyzed by the current method. No sample was found to exceed the permitted level.
关 键 词:高效毛细管区带电泳 三氯蔗糖 间接紫外法 3 5-二硝基苯甲酸 食品添加剂 食品安全
分 类 号:R155.5[医药卫生—营养与食品卫生学]
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