首页|高效液相色谱法测定涂料中3种含氟烷基丙烯酸酯化合物的含量

高效液相色谱法测定涂料中3种含氟烷基丙烯酸酯化合物的含量

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取2.000 g涂料样品,加入15 mL乙腈,涡旋30 s,于30 ℃超声萃取40 min.冷却至室温,用乙腈定容至20 mL.分取1 mL,过0.22 μm滤膜,滤液进入高效液相色谱仪,在ZORBAX SB-Aq色谱柱上以不同体积比的乙腈和水的混合溶液梯度洗脱分离3种含氟烷基丙烯酸酯化合物(FTAs)全氟辛基乙基丙烯酸酯(8∶2FTA)、全氟癸基乙基丙烯酸酯(10∶2FTA)和全氟己基乙基丙烯酸酯(6∶2 FTA),外标法定量.结果显示,3种FTAs的质量浓度在0.2~5.0mg·L-1内和峰面积呈线性关系,检出限(3S/N)为0.27~0.34 mg·kg-1.按照标准加入法进行回收试验,回收率为93.5%~109%,测定值的相对标准偏差(n=6)为0.50%~4.7%.方法用于10款涂料样品的分析,在2款样品中检出了 8∶2 FTA,检出量分别为 226.7 mg·kg-1 和4.1 mg·kg-1.
Determination of 3 Fluoroalkyl Acrylate Compounds in Coating by High Performance Liquid Chromatography
The 2.000 g of coating sample was taken,and 15 mL of acetonitrile was added.The mixture was vortexed for 30 s,and extracted by ultrasound at 30 ℃ for 40 min.After cooling to room temperature,the extract was made its volume up to 20 mL with acetonitrile.An aliquot(1 mL)was taken,and passed through a 0.22 μm filter membrane,and the filtrate was introduced into a high performance liquid chromatograph.Three fluoroalkyl acrylate compounds(FTAs),including 1H,1H,2H,2H-perfluorodecyl acrylate(8∶2 FTA),1H,1H,2H,2H-perfluorododecyl acrylate(10∶2 FTA),and 1H,1H,2H,2H-perfluorooctyl acrylate(6∶2 FTA)were separated on a ZORBAX SB-Aq column by gradient elution with a mixture of acetonitrile and water at different volume ratios,with external standard method for quantification.It was shown that linear relationships between values of mass concentration and peak area of the 3 FTAs were kept in the range of 0.2-5.0 mg·L-1,and the detection limits(3S/N)were found in the range of 0.27-0.34 mg·kg.Test for recovery was made according to the standard addition method,giving recoveries in the range of 93.5%-109%,with RSDs(n=6)of the determined values ranged from 0.50%to 4.7%.The proposed method was used for the analysis of 10 types of coating samples,and 8∶2 FTA was detected in two types of samples,with detection amounts of 226.7 mg·kg-1 and 4.1 mg·kg-1,respectively.

fluoroalkyl acrylate compoundhigh performance liquid chromatographycoating

李支薇、张兰兰、李勇、钟琳、秦宇媚

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广电计量检测集团股份有限公司,广州 510700

中车长春轨道客车股份有限公司,长春 130062

广东省大湾区华南理工大学聚集诱导发光高等研究院,广州 510700

含氟烷基丙烯酸酯化合物 高效液相色谱法 涂料

2024

理化检验-化学分册
上海材料研究所

理化检验-化学分册

CSTPCD北大核心
影响因子:0.647
ISSN:1001-4020
年,卷(期):2024.60(12)