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镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取

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丁炜楠, 刘婷婷, 赵丹青, 顾海东, 张占恩. 镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取[J]. 环境化学, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
引用本文: 丁炜楠, 刘婷婷, 赵丹青, 顾海东, 张占恩. 镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取[J]. 环境化学, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
shu
DING Weinan, LIU Tingting, ZHAO Danqing, GU Haidong, ZHANG Zhanen. One-pot preparation method of nickel and nitrogen co-doped carbon nanotubes and its extraction of estrogen in milk samples[J]. Environmental Chemistry, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
Citation: DING Weinan, LIU Tingting, ZHAO Danqing, GU Haidong, ZHANG Zhanen. One-pot preparation method of nickel and nitrogen co-doped carbon nanotubes and its extraction of estrogen in milk samples[J]. Environmental Chemistry, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
shu

镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取

  • 苏州科技大学环境科学与工程学院, 苏州, 215009

    • 通讯作者: 张占恩, E-mail: ustswxd@163.com
  • 基金项目:

    科技部国家重点研发计划（2017YFC0211903）资助.

One-pot preparation method of nickel and nitrogen co-doped carbon nanotubes and its extraction of estrogen in milk samples

  • School of Environmental Science and Engineering, Suzhou University of Science and Technology, Suzhou, 215009, China

    • Corresponding author: ZHANG Zhanen, ustswxd@163.com
  • Fund Project: Supported by the National Key R&D Program of China (2017YFC0211903).

  • 摘要: 利用高温煅烧法一步合成制备了磁性镍、氮共掺杂碳纳米管（Ni@N-CNTs）并将其与泡腾片剂结合应用于牛奶中4种雌激素的萃取.研究了萃取剂的质量，pH，洗脱剂种类及体积等对萃取回收率的影响，并通过磁固相萃取结合高效液相色谱法将其成功用于牛奶中雌二醇、雌酮、己烯雌酚和己烷雌酚等4种雌激素的检测.该方法对雌二醇和己烷雌酚的线性范围为1.0—500.0 μg·L-1，对雌酮和己烯雌酚的线性范围为2.0—500.0 μg·L-1，4种物质检出限为0.24—0.50 μg·L-1，日内日间精密度分别为3.18%—4.96%和4.54%—6.32%.牛奶样品中回收率为85.2%—102.9%.因此，建立的方法在微萃取领域有很大的应用前景.
    Abstract: In this study, Ni@N-CNTs co-doped with nickel nanoparticles and nitrogen atoms were prepared by one-step synthesis by high-temperature calcination. Ni@N-CNTs were used for effervescent reaction to assist the dispersion of magnetic solid-phase extraction of estrogens in milk. Among them, Ni particles provided magnetic properties, nitrogen atoms provided adsorption sites, and the tubular structure of the material provided a larger contact surface area, and the effervescent reaction is used to make the material fully contact with estrogens. And the effect of extractant quality, pH, type and volume of the eluent on the extraction recovery was then optimized. Finally, four factors of estradiol, estrone, diethylstilbestrol, and hexestrol in milk were successfully detected by MSPE combined with high-performance liquid chromatography. The linear range of estradiol and hexestrol was 1.0-500.0 μg·L-1, the linear range of estrone and diethylstilbestrol was 2.0-500.0 μg·L-1, and the detection limit of 4 substances was 0.24. 0.50 μg·L-1, relative standard deviations (RSDs) for inter-day (n=6) and intra-day (n=3) were 3.18%-4.96% and 4.54%-6.32%, respectively. The recovery of milk samples ranged from 85.2% to 102.9%. Therefore, this study had great application prospects in the field of micro-extraction.
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  • 收稿日期:  2019-08-07
丁炜楠, 刘婷婷, 赵丹青, 顾海东, 张占恩. 镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取[J]. 环境化学, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
引用本文: 丁炜楠, 刘婷婷, 赵丹青, 顾海东, 张占恩. 镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取[J]. 环境化学, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
shu
DING Weinan, LIU Tingting, ZHAO Danqing, GU Haidong, ZHANG Zhanen. One-pot preparation method of nickel and nitrogen co-doped carbon nanotubes and its extraction of estrogen in milk samples[J]. Environmental Chemistry, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
Citation: DING Weinan, LIU Tingting, ZHAO Danqing, GU Haidong, ZHANG Zhanen. One-pot preparation method of nickel and nitrogen co-doped carbon nanotubes and its extraction of estrogen in milk samples[J]. Environmental Chemistry, 2020, (5): 1420-1426. doi: 10.7524/j.issn.0254-6108.2019080703
shu

镍、氮共掺杂碳纳米管的一锅制备法及其对牛奶样品中雌激素的萃取

    通讯作者: 张占恩, E-mail: ustswxd@163.com
  • 苏州科技大学环境科学与工程学院, 苏州, 215009
  • 收稿日期:  2019-08-07
基金项目:

科技部国家重点研发计划（2017YFC0211903）资助.

摘要: 利用高温煅烧法一步合成制备了磁性镍、氮共掺杂碳纳米管（Ni@N-CNTs）并将其与泡腾片剂结合应用于牛奶中4种雌激素的萃取.研究了萃取剂的质量，pH，洗脱剂种类及体积等对萃取回收率的影响，并通过磁固相萃取结合高效液相色谱法将其成功用于牛奶中雌二醇、雌酮、己烯雌酚和己烷雌酚等4种雌激素的检测.该方法对雌二醇和己烷雌酚的线性范围为1.0—500.0 μg·L-1，对雌酮和己烯雌酚的线性范围为2.0—500.0 μg·L-1，4种物质检出限为0.24—0.50 μg·L-1，日内日间精密度分别为3.18%—4.96%和4.54%—6.32%.牛奶样品中回收率为85.2%—102.9%.因此，建立的方法在微萃取领域有很大的应用前景.

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