浊点萃取-高效液相色谱法同时测定烟用接装纸中可萃取Cr(Ⅲ)和Cr(Ⅵ)

Simultaneous determination of extractable Cr(Ⅲ)and Cr(Ⅵ)in cigarette tipping paper by cloudpoint extraction-high performance liquid chromatography method

建立同时测定烟用接装纸中可萃取Cr(Ⅲ)和Cr(Ⅵ)的方法——浊点萃取-高效液相色谱法(cloudpoint extraction-high performance liquid chromatography,CPE-HPLC)。该方法用超纯水超声萃取接装纸样品30 min,pH为5.0,温度55℃条件下,以吡咯烷二硫代甲酸铵(ammonium pyrrolidine dithiocarbamate,APDC)为螯合剂,曲拉通(Triton)X-114非离子表面活性剂为萃取剂,同时富集溶液中的Cr(Ⅲ)和Cr(Ⅵ),用HPLC分离并测定。结果显示,Cr(Ⅲ)回收率为96.2%~103.6%,RSD为4.6%~7.1%,Cr(Ⅵ)回收率为94.7%~104.4%,RSD为4.3%~8.5%,Cr(Ⅲ)和Cr(Ⅵ)的富集因子分别为15.3和20.1,检出限分别为14μg/kg和10μg/kg。该方法检测灵敏度高,检出限低,稳定性好,具有良好的精密度、回收率和较高的富集倍数,适用于烟用接装纸中可萃取Cr(Ⅲ)和Cr(Ⅵ)的同时测定。

A method was established for the simultaneous determination of extractable Cr(Ⅲ)and Cr(Ⅵ)in cigarette tipping paper based on cloudpoint extraction(CPE)by High performance liquid chromatography(HPLC).The samples were reacted with ammonium pyrrolidine dithioformate(APDC)at 55℃and pH 5.0 affter extracted by ultrasonic extraction with ultrapure water for 30 min,then determined by HPLC affter extracted by Triton X-114.The results show that,recovery of Cr(Ⅲ)was 96.2%-103.6%,RSD was 4.6%-7.1%;recovery of Cr(Ⅵ)was 94.7%-104.4%,RSD was 4.3%-8.5%.the enrichment factors of Cr(Ⅲ)and Cr(Ⅵ)were 15.3 and 20.1,the detection limits were 14μg/kg and 10μg/kg.The method is suitable for the simultaneous determination of extractable Cr(Ⅲ)and Cr(Ⅵ)in cigarette tipping paper because of its sensitivity,detection limit,stability,precision,recovery and high enrichment ratio.