高效液相色谱法测定水性涂料中碘丙炔醇丁基氨甲酸酯和吡啶硫酮锌的含量
Determination of Iodopropynyl Butylcarbamate and Zinc Pyrithione in Water-Borne Coating by High Performance Liquid Chromatography
张琳 1杨娟 1郭争云 1徐骏 1程欲晓1
作者信息
- 1. 上海海关工业品与原材料检测技术中心,上海 200135
- 折叠
摘要
取涂料样品约2 g,用10 mL N,N-二甲基甲酰胺(DMF)超声萃取10 min,冷却至室温,离心5 min,取上清液至50 mL容量瓶中.残余物用10 mL乙腈超声萃取10 min,离心5 min,重复2次,合并上清液,用乙腈定容至50 mL.所得溶液经0.22 μm亲水聚四氟乙烯(PTFE)滤膜过滤,在Agilent ZORBAX Eclipse Plus C18柱上进行分离,以体积比7:3的乙腈-[10 mmol·L-1磷酸二氢钾-1.0 mmol·L-1乙二胺四乙酸二钠(Na2EDTA)溶液(pH 4.0)]混合液为流动相进行等度洗脱,采用高效液相色谱法(HPLC)测定其中碘丙炔醇丁基氨甲酸酯(IPBC)和吡啶硫酮锌(ZPT)的含量,检测波长为235 nm.结果表明,IPBC和ZPT标准曲线的线性范围分别为20～2 000 mg·L-1 和 50～800 mg·L-1,检出限(3S/N)分别为 106,298 mg·kg-1.按照标准加入法进行回收试验,回收率为92.4％～103％,测定值的相对标准偏差(n=6)均小于3.0％.方法用于4种实际样品的分析,仅一种室内用水性涂料检出ZPT,检出量为920 mg·kg-1.
Abstract
The coating sample(about 2 g)was taken,ultrasonically extracted with 10 mL of N,N-dimethylformamide(DMF)for 10 min,cooled to room temperature,and centrifuged for 5 min.The supernatant was taken to a 50 mL-volumetric flask.The residue was ultrasonically extracted with 10 mL of acetonitrile for 10 min,and centrifuged for 5 min.After repeated twice,the supernatants were combined,and made its volume up to 50 mL with acetonitrile.The obtained solution was passed through 0.22 μm hydrophilic polytetrafluoroethylene(PTFE)filtration membrane,and separated on Agilent ZORBAX Eclipse Plus C18 column,using a mixture of acetonitrile and 10 mmol·L-1 potassium dihydrogen phosphate-1.0 mmol·L-1 Na2EDTA solution(pH 4.0)at a volume ratio of 7:3 as the mobile phase for isocratic elution.Iodopropynyl butylcarbamate(IPBC)and zinc pyrithione(ZPT)were determined by high performance liquid chromatography(HPLC),with detection wavelength of 235 nm.As shown by the results,linear ranges of the IPBC and ZPT standard curves were 20-2 000 mg·L-1 and 50-800 mg·L-1,with detection limits(3S/N)of 106,298 mg·kg-1,respectively.Test for recovery was made by the standard addition method,giving the results in the range of 92.4％-103％,with RSDs(n=6)of the determined values less than 3.0％.This method was used for the analysis of 4 actual samples,and ZPT was detected in only one indoor water-borne coating,with detection amount of 920 mg·kg-1.
关键词
高效液相色谱法(HPLC)/吡啶硫酮锌(ZPT)/碘丙炔醇丁基氨甲酸酯(IPBC)/水性涂料Key words
high performance liquid chromatography(HPLC)/zinc pyrithione(ZPT)/iodopropynyl butylcarbamate(IPBC)/water-borne coating引用本文复制引用
出版年
2023
NETL
NSTL
维普
万方数据