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作 者:丁晓静[1,2,3] 刘文叶 王萍[1,2] DING Xiaojing;LIU Wenye;WANG Ping(Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Control and Prevention,Beijing 100013,China;Beijing Research Center for Preventive Medicine Research,Beijing 100013,China;School of Public Health,Capital Medical University,Beijing 100069,China)
机构地区:[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 处:《食品科学》2020年第4期287-292,共6页Food Science
基 金: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);国家重点研发计划“国家质量基础的共性技术研究与应用”重点专项(2016YFF0201106)
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75μm×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5μg/L和15μg/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0.9999。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。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 75μm×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 0.9999 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 15μg/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-fl uorescence detection(UPLC-FLR).The possible reasons for the difference were analyzed and discussed.
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