| 高效液相色谱-荧光检测法测定塑料儿童玩具中苯并唑类荧光增白剂 |
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| 基金项目:国家重点研发计划(2016YFF0103800,2016YFF0203701)；湖南省创新平台与人才计划(2017RS3055)；长株潭国家自主创新示范区专项(2018XK2006-1) |
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| 中文摘要:建立了高效液相色谱-荧光检测法同时测定塑料儿童玩具中4种苯并唑类荧光增白剂(FWA 135、FWA 367、FWA 368、FWA 184)的方法。样品经粉碎后，采用20 mL乙腈-三氯甲烷(6∶4，体积比)混合溶液一步溶剂提取法对样品进行前处理，40 ℃下超声提取30 min后，进行高效液相色谱分析。以乙腈和水作为流动相，Waters SunFire C18色谱柱梯度洗脱，荧光激发波长(Ex)为360 nm，发射波长(Em)为430 nm。结果显示，FWA 135在1~100 μg/L质量浓度范围内具有良好的线性关系，其他3种荧光增白剂在2~200 μg/L质量浓度范围内线性关系良好，相关系数(r2)均不小于0.999 3，检出限分别为0.5、1、1、1 μg/L。加标水平为0.1、0.4、2.0 mg/kg时，4种荧光增白剂的回收率为84.2%~106%，相对标准偏差均小于10%。对市售10种儿童玩具进行检测，部分样品中4种苯并唑类荧光增白剂均有检出。该方法操作简单，回收率好，精密度高，适用于各种类型塑料儿童玩具中上述荧光增白剂的测定。 |
| 中文关键词:高效液相色谱（HPLC） 荧光检测 苯并唑类 荧光增白剂 儿童玩具 |
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| Determination of Benzoxazole Fluorescent Whitening Agents in Plastic Children's Toys by High Performance Liquid Chromatography with Fluorescence Detector |
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| Abstract:A high performance liquid chromatography with fluorescence detector was developed for the simultaneous determination of four benzoxazole fluorescent whitening agents,i.e.FWA 135,FWA 367,FWA 368 and FWA 184 in plastic children's toys.The sample was crushed and pretreated with 20 mL acetonitrile-chloroform(6∶4,by volume) mixed solution by one step solvent extraction,then ultrasonically extracted at 40 ℃ for 30 min,and finally analyzed by HPLC with fluorescence detection.The extract was separated on a Waters SunFire C18 column by gradient elution with acetonitrile and water as mobile phases.The fluorescence excitation wavelength(Ex) was set at 360 nm,and the emission wavelength(Em) was 430 nm.Results showed that the calibration curves were linear(r2≥0.999 3) in the range of 1-100 μg/L for FWA 135,and 2-200 μg/L for the other three fluorescent whitening agents.The detection limits for FWA 135,FWA 367,FWA 368 and FWA 184 were 0.5,1,1 and 1 μg/L,respectively.The recoveries for four fluorescent whitening agents at three spiked levels of 0.1,0.4 and 2.0 mg/kg ranged from 84.2% to 106%,with relative standard deviations less than 10%.Ten kinds of childrens toys were tested,and four kinds of benzoxazole fluorescent whitening agents were detected.With the advantages of simple operation,good recovery and high precision,the method is applicable for the determination of the fluorescent whitening agents in various types of children's toys. |
| Key Words:high performance liquid chromatography(HPLC) fluorescence detection benzoxazoles fluorescent whitening agents children's toys |
| 引用本文：周雯鹂，陈茂龙，许宙，朱绍华，丁利.高效液相色谱-荧光检测法测定塑料儿童玩具中苯并唑类荧光增白剂[J].分析测试学报,2020,39(9):1137-1142. |
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