摘要
建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定棉、羊毛、涤纶等纺织品中1H,1H,2H,2H-全氟-1-己醇(4∶2 FTOH)、1H,1H,2H,2H-全氟-1-辛醇(6∶2 FTOH)、1H,1H,2H,2H-全氟-1-癸醇(8∶2 FTOH)、1H,1H,2H,2H-全氟-1-十二烷醇(10∶2 FTOH)4种全氟烷基醇(FTOHs)的分析方法。样品用甲醇超声波提取,HLB固相萃取柱净化后,采用Acquity UPLC BEH-C18色谱柱(50 mm×2.1 mm,1.7μm)分离,以甲醇-0.01%氨水溶液为流动相梯度洗脱,质谱采用电喷雾电离,负离子扫描,多反应监测(MRM)模式进行检测,外标法定量。结果表明:4种目标物的定量限(LOQ,以信噪比>10计)为0.01~0.1 mg/kg,线性相关系数均大于0.99,回收率为84.1%~99.0%,相对标准偏差(RSD)为3.7%~8.9%。该方法快速、操作简便、灵敏高,适用于纺织品中FTOHs的定量和确证分析。
A new method for determination of 4 perfluoroalkyl alcohols(including 1 H,1 H,2 H,2 H-Perfluoro-1-hexanol(4∶2 FTOH),1 H,1 H,2 H,2 H-Perfluoro-1-octanol(6∶2 FTOH),1 H,1 H,2 H,2 H-Perfluoro-1-decanol(8∶2 FTOH) and 1 H,1 H,2 H,2 H-Perfluoro-1-dodecanol(10∶2 FTOH) in textiles by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed.The textiles were extracted by ultrasonic technique for 30 min with methanol,then cleaned up by HLB solid phase extraction column.The separation was performed on Acquity UPLC BEH-C18 column(50×2.1 mm,1.7 μm) with gradient elution using acetonitrile-0.01% aqueous ammonia,then analyzed in negative ions with multiple reaction monitoring(MRM) mode.The results showed that the limits of quantification(LOQ,S/N>10) were in range of 0.01-0.1 mg/kg,the linear correlation coefficients were all more than 0.99.The recoveries of 4 perfluoroalkyl alcohols ranged from 84.1% to 99.0% with relative standard deviations of 3.7%-8.9%.The method is rapid,simple and sensitive,and suitable for quantitative and confirmatory analysis of perfluoroalkyl alcohols in textiles.
作者
刘海山
奚君阳
汤杭燕
李丹
李新宇
LIU Hai-shan;XI Jun-yang;TANG Hang-yan;LI Dan;LI Xin-yu(Technology Center of Hangzhou Customs District,Hangzhou 311215;Zhejiang Academy of Science&Technology for Inspection&Quarantine,Hangzhou 311215)
出处
《分析科学学报》
CAS
CSCD
北大核心
2019年第6期836-840,共5页
Journal of Analytical Science
基金
原国家质量监督检验检疫总局科技计划(No.2017IK181)
关键词
超高效液相色谱-串联质谱
测定
纺织品
全氟烷基醇
Ultra-high performance liquid chromatography-tandem mass spectrometry
Determination
Textiles
Perfluoroalkyl alcohols
