食品科学 ›› 2020, Vol. 41 ›› Issue (4): 287-292.doi: 10.7506/spkx1002-6630-20190101-006

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胶束电动毛细管色谱-激光诱导荧光检测法测定番茄酱、番茄沙司和辣椒粉中罗丹明B

丁晓静,刘文叶,王萍   

  1. (1.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,北京 100013;2.北京市预防医学研究中心,北京 100013;3.首都医科大学公共卫生学院,北京 100069)
  • 出版日期:2020-02-25 发布日期:2020-03-02
  • 基金资助:
    北京市卫生系统高层次卫生技术人才培养计划项目(2013-2-036);

Determination of Rhodamine B in Ketchup, Tomato Sauce and Chili Powder by Micellar Electrokinetic Capillary Chromatography with Laser-Induced Fluorescence Detection

DING Xiaojing, LIU Wenye, WANG Ping   

  1. (1. Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention, Beijing 100013, China; 2. Beijing Research Center for Preventive Medicine Research, Beijing 100013, China; 3. School of Public Health, Capital Medical University, Beijing 100069, China)
  • Online:2020-02-25 Published:2020-03-02

摘要: 建立食品中非食用色素罗丹明B的胶束电动毛细管色谱-激光诱导荧光检测方法。以75 μm×30 cm(有效长度为20 cm)未涂层熔融石英毛细管为分离柱;以30 mmol/L Na2B4O7+20 mmol/L十二烷基硫酸钠(sodium sodecyl sulfonate,SDS)+20 mmol/L脱氧胆酸钠+0.2 g/L聚乙二醇35000为分离缓冲溶液,10 mmol/L SDS为样品提取液,在10 min内即可实现罗丹明B的测定。分离电压8 kV、进样压力3.448 kPa、时间5 s,激发波长488 nm,发射波长520 nm。检出限和定量限分别为5 μg/L和15 μg/L。在0.02~1.28 mg/L范围内,罗丹明B的校正峰面积与质量浓度呈良好线性关系,相关系数为0.999 9。方法日内及日间精密度相对标准偏差均不高于2%。低、中和高添加水平(0.04、0.16、0.64 mg/L)的加标回收率在100.9%~105.8%之间。用该方法测定3 个番茄酱样品、3 个番茄沙司样品和22 个辣椒粉样品,胶束电动毛细管色谱-激光诱导荧光法检测结果均比超高效液相色谱-荧光检测法结果偏低,对可能的原因进行了分析。

关键词: 胶束电动毛细管色谱, 激光诱导荧光, 罗丹明B, 番茄酱, 番茄沙司, 辣椒粉

Abstract: A new and simple method was developed for the accurate determination of rhodamine B in ketchup, tomato sauce and chili powder samples by micellar electrokinetic capillary chromatography (MEKC) with laser-induced fluorescence (LIF) detection. The separation was performed on an uncoated fused silica capillary 75 μm × 30 cm total length (effective length: 20 cm) with a separation buffer solution consisting of 30 mmol/L sodium tetraborate, 20 mmol/L sodium dodecyl sulfonate (SDS), 20 mmol/L sodium deoxycholate (SD) and 0.2 g/L polyethyleneglycol 35000. A solution containing 10 mmol/L SDS was used for sample extraction. The analysis could be completed within 10 min. A voltage of 8 kV was used for separation. The injection time and pressure were 5 s and 3.448 kPa, respectively. The excitation and emission wavelengths were 488 nm and 520 nm, respectively. The corrected peak area and the concentration of rhodamine B displayed a good linear relationship with a correlation coefficient (r) of 0.999 9 in the ranges of 0.02–1.28 mg/L. The limit of detection (LOD; RSN = 3) and limit of quantitation (LOQ; RSN = 10) were 5 and 15 μg/L, respectively. The intra-day and inter-day precisions of the method were both no less than 2%. The average recoveries of rhodamine B at three spiked concentrations (0.04, 0.16 and 0.64 mg/L) were in the ranges of 100.9%–105.8%. When the MEKC method was used to determine the contents of rhodamine B in 3 ketchup, 3 tomato sauce and 22 chili powder samples, the results were all lower than those measured by ultra-high performance liquid chromatography-fluorescence detection (UPLC-FLR). The possible reasons for the difference were analyzed and discussed.

Key words: micellar electrokinetic chromatography, laser-induced fluorescence, rhodamine B, sauce, ketchup, chili powder

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