毛细管区带电泳-间接紫外测定食品中木糖醇
目的 建立毛细管区带电泳间接紫外测定食品中木糖醇的新方法。方法 样品用超纯水提取后离心, 过0.45 μm膜后上机进样。以未涂敷熔融石英毛细管(50 μm×60.2 cm)为毛细管分离柱, 以8 mmol/L 3, 5-二硝基苯甲酸、10 mmol/L硼砂和0.5 mmol/L十六烷基三甲基溴化铵为分离缓冲溶液。分离电压为-20 kV, 检测波长为200 nm, 用外标法定量。结果 方法检出限为3.00 mg/L(S/N=3), 定量限为10.00 mg/L (S/N=9), 线性范围为10.00~300.0 mg/L, 线性相关系数r为0.9994。在20.00、40.00、80.00 mg/L添加水平下, 平均回收率分别为103.2%、103.3%及104.8%, 相对标准偏差分别为0.5%、1.2%及0.7%(n=3)。结论 该方法简单快速, 11 min内即可完成一次样品分析(清洗6 min、分离5 min), 试剂及样品消耗量少, 适用于食品中木糖醇的检测。
Objective To develop a new method for the detection of xylitol in food by capillary zone electrophoresis with indirect ultraviolet. Methods Samples were extracted with ultrapure water, centrifuged and injected by 0.45 μm membrane. The separation was carried out using an uncoated fused-silica capillary with 50 μm i.d. and 60.2 cm total length. The separation buffer consisted of 8 mmol/L 3, 5-dinitrobenzoic acid, 10 mmol/L sodium tetraborate and 0.5 mmol/L hexadecyl trimethyl ammonium bromide, separation voltage was -20 kV and the detection wavelength was 200 nm. Quantification was made by external calibration between the corrected peak area and the concentration of xylitol. Results The limit of detection and limit of quantitation were 3.00 mg/L (S/N=3) and 10.00 mg/L (S/N=9), respectively. The linear range between the corrected peak area and the concentration was from 10.00 to 300.0 mg/L with a correlation coefficient of 0.9994. The average spiked recoveries of 3 levels (20.00, 40.00 and 80.00 mg/L) were 103.2, 103.3 and 104.8% with relative standard deviations of 0.5%, 1.2% and 0.7%, respectively. Conclusion The method is simple and fast and the analysis could be completed within 11 min (6 min for rinsing and 5 min for separation), which is suitable for the determination of xylitol in food samples.
标题：毛细管区带电泳-间接紫外测定食品中木糖醇
英文标题：Determination of xylitol by capillary zone electrophoresis with indirect ul-traviolet detection in food
作者：
李疆 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室
陈桐 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,首都医科大学附属北京安贞医院,首都医科大学公共卫生学院
鞠昭函 北京联合大学应用文理学院
赵珊 北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室
丁晓静 北京市疾病预防控制中,食物中毒诊断溯源技术北京市重点实验室;首都医科大学公共卫生学院
中文关键词:毛细管区带电泳,间接紫外法,木糖醇,3, 5-二硝基苯甲酸,
英文关键词:capillary zone electrophoresis,indirect ultraviolet detection,xylitol,3, 5-dinitrobenzoic acid,
发表日期：2015-12-14
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