| 高效液相色谱-荧光法同时测定食品接触纸制品中15种荧光增白剂 |
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| 基金项目:国家重点研发计划项目(2016YFF0203705)；广州海关科研项目(2020GZCK-026) |
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| 中文摘要:建立了高效液相色谱-荧光法同时测定食品接触纸制品中15种荧光增白剂的分析方法，测定对象包括离子型和非离子型荧光增白剂，其中包括部分同分异构体。样品经切碎后，采用一步溶剂提取法利用碱性提取液对样品中的荧光增白剂进行超声提取，提取液过膜后进行高效液相色谱分析。以乙腈、甲醇和四丁基溴化铵甲醇水溶液作为流动相，Agilent Pursuit 5 PFP(4.6 mm×250 mm×5.0 μm)为色谱柱进行梯度洗脱。结果表明，15种荧光增白剂在一定质量浓度范围内线性关系良好，相关系数(r)均不小于 0.998 9，检出限为0.030~0.60 mg/kg，定量下限为0.10~2.0 mg/kg。在3个加标水平下，15种荧光增白剂的回收率为90.0%~108%，相对标准偏差为0.70%~7.1%。所建立的方法成功应用于市售13种食品接触纸制品中荧光增白剂含量的测定，证明该方法实用性强，操作简便，灵敏度高。 |
| 中文关键词:荧光增白剂 食品接触纸制品 高效液相色谱 荧光检测 |
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| Simultaneous Determination of 15 Fluorescent Whitening Agents in Food Contact Paper Products by High Performance Liquid Chromatography Coupled with Fluorescence Detection |
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| Abstract:A high performance liquid chromatography(HPLC) with fluorescence detection based on a simple pretreatment method was established for the simultaneous determination of 15 kinds of fluorescent whitening agents in food contact paper products,with widely used and low-cost ionic fluorescent whitening agents as well as some fluorescent whitening agents such as fluorescent whitening agent 393 and fluorescent whitening agent 184 concerned in the European Union and China as the research objects.The analysis objects included ionic and non-ionic fluorescent whitening agents,some of which were isomers,including ionic fluorescent whitening agents 220 and 24,and non-ionic fluorescent whitening agents 199A and 199B.At present,the chromatographic analysis methods for fluorescent whitening agents are mainly corresponding to ionic and non-ionic fluorescent whitening agents,and the chromatographic separations are mainly carried out with C18 column.However,there are few studies on simultaneous determination of the two types of fluorescent whitening agents and some of their isomers.In that case,a series of parameters such as chromatographic column,mobile phase,flow rate,pH value and elution gradient were optimized in this paper to achieve the chromatographic separation and simultaneous detection of 15 fluorescent whitening agents.Consequently,the samples were separated using an Agilent Pursuit 5 PFP(4.6 mm×250 mm×5.0 μm) by gradient elution,with acetonitrile,methanol and the solution of tetrabutyl ammonium bromide as the mobile phases.In the pretreatment process,the extraction solvent,extraction time,extraction volume and separation method were optimized to realize the effective extraction of fluorescent whitening agents from food contact paper products.Specifically,during the analysis process,the samples were crushed,and the one-step solvent extraction was applied to extract the fluorescent whitening agents in samples with alkaline extract solution through ultrasonic process.Subsequently,the extract solution was filtrated,and analyzed by high performance liquid chromatography.Results showed that there were good linear relationships for the calibration curves of 15 fluorescent whitening agents,with their correlation coefficients(r) not less than 0.998 9.The limits of detection and the limits of quantitation were in the ranges of 0.030-0.60 mg/kg and 0.10-2.0 mg/kg,respectively.Under the detection limited concentrations set in this paper,15 kinds of fluorescent whitening agents were found to exhibit no obvious fluorescence phenomenon by ultraviolet light illumination method,which indicated that the method reached a high sensitivity.The recoveries for 15 fluorescent whitening agents at three spiked levels ranged from 90.0% to 108%,with relative standard deviations of 0.70%-7.1%.The established method was successfully used for the determination of 13 commercial paper products with good practicability,simplicity and sensitivity.The establishment of this method could realize the further identification of the types and contents of fluorescent whitening agents in food contact paper with positive fluorescence phenomenon,which has a certain guiding significance for the quality and safety management and control of food contact paper products. |
| Key Words:fluorescent whitening agents food contact paper products high performance liquid chromatography fluorescence detection |
| 引用本文：梁瑞钰,黎梓城,汪龙飞,鲍蕾,李丹,潘静静,钟怀宁,郑建国.高效液相色谱-荧光法同时测定食品接触纸制品中15种荧光增白剂[J].分析测试学报,2021,40(6):934-939. |
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