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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)

353    2022-09-15

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作者:王洋, 韩维岐, 郭莉莉, 金哲

作者单位:吉林烟草工业有限责任公司技术研发中心,吉林 长春 130000


关键词:浊点萃取(CPE);高效液相色谱法(HPLC);烟用接装纸;三价铬;六价铬


摘要:

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14 μg/kg和10 μg/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。


Simultaneous determination of extractable Cr(Ⅲ) and Cr(Ⅵ) in cigarette tipping paper by cloudpoint extraction-high performance liquid chromatography method
WANG Yang, HAN Weiqi, GUO Lili, JIN Zhe
Technology R & D Center of Jilin Tobacco Industrial Co., Ltd., Changchun 130000, China
Abstract: 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 14 μg/kg and 10 μg/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.
Keywords: cloudpoint extraction(CPE);high performance liquid chromatography(HPLC);cigarette tipping paper;Cr(Ⅲ);Cr(Ⅵ)
2022, 48(7):72-76,106  收稿日期: 2021-11-15;收到修改稿日期: 2022-02-22
基金项目:
作者简介: 王洋(1986-),女,吉林白城市人,工程师,硕士,主要从事卷烟化学研究
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