高等学校化学学报 ›› 2019, Vol. 40 ›› Issue (5): 901-908.doi: 10.7503/cjcu20180531

• 分析化学 • 上一篇    下一篇

SiW11掺杂二氧化硅纳米纤维(SiW11/SiO2)的制备及对拟南芥叶中多胺的萃取分析

蔡娇, 余琼卫, 何小梅, 许静, 丁琼, 冯钰锜()   

  1. 生物医学分析化学教育部重点实验室, 武汉大学化学与分子科学学院, 武汉 430072
  • 收稿日期:2018-07-27 出版日期:2019-04-18 发布日期:2019-04-18
  • 作者简介:

    联系人简介: 冯钰锜, 男, 博士, 教授, 博士生导师, 主要从事色谱质谱分析研究. E-mail: yqfeng@whu.edu.cn

  • 基金资助:
    国家自然科学基金(批准号: 31671929, 31670373)资助.

Preparation of SiW11 Incorporated SiO2 Nanofibers(SiW11/SiO2) and Its Application in the Analysis of Polyamines in Arabidopsis

CAI Jiao, YU Qiongwei, HE Xiaomei, XU Jing, DING Qiong, FENG Yuqi*()   

  1. Key Laboratory of Analytical Chemistry for Biology and Medicine, Ministry of Education, College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • Received:2018-07-27 Online:2019-04-18 Published:2019-04-18
  • Contact: FENG Yuqi E-mail:yqfeng@whu.edu.cn
  • Supported by:
    † Supported by the National Natural Science Foundation of China(Nos.31671929, 31670373).

摘要:

采用静电纺丝技术制备了SiW11掺杂的二氧化硅纳米纤维(SiW11/SiO2)材料, 其中掺杂的SiW11质量占纤维质量的7.83%, 制备的SiW11/SiO2材料尺寸均一, 在考察的pH范围内带负电, 与未掺杂SiW11的二氧化硅纳米纤维相比, SiW11/SiO2材料表现出强阳离子交换作用, 能有效萃取尸胺和腐胺. 在最优条件下, 建立了注射器分散固相萃取(In syringe dSPE)-超高效液相色谱-串联质谱联用(UHPLC-MS/MS)检测拟南芥样品中多胺的方法. 结果表明, 尸胺和腐胺分别在10~1000和20~1000 ng/mL浓度范围内具有良好的线性关系(R2≥0.9950), 检出限和定量限分别为0.5~0.9和1.6~3.0 ng/mL. 将该方法应用于拟南芥样品中尸胺和腐胺的检测, 加标回收率在87.5%~111.3%之间, 相对标准偏差RSD<5.0%. 建立的SiW11/SiO2制备方法解决了多金属氧酸盐(POM)在修饰改性过程中存在的制备繁琐、 固载量少的问题, 拓宽了POM在分离领域中的应用.

关键词: 多金属氧酸盐, SiW11/SiO2, 静电纺丝, 注射器分散固相萃取, 多胺

Abstract:

SiW11 incorporated SiO2 nanofibers(SiW11/SiO2) was prepared by electrospinning technology. The mass of incorporated SiW11 accounted for 7.83% of nanofibers. SiW11/SiO2 nanofiber possessed uniform structure with the diameter about 450 nm, and was negative charged in the pH range of 1.0—11.0. Compared with SiO2 nanofibers, the SiW11/SiO2 nanofiber exhibited stronger cation-exchange interactions to extract PUT and CAD. Under the optimized condition, an in-syringe dSPE-UHPLC-MS/MS method for rapid and selective detection of polyamines from plants was established. The limits of detection(LODs) for the target CAD and PUT ranged from 0.5 ng/mL to 0.9 ng/mL, and the linear range was 10—1000 ng/mL and 20—1000 ng/mL with determination coefficients(R2) higher than 0.9950. The recoveries ranged from 87.5% to 111.3% with relative standard deviations(RSDs) of 1.9%—7.2%. The proposed method can be used to detect the trace CAD and PUT in Arabidopsis.

Key words: Polyoxometalate(POM), SiW11/SiO2, Electrospinning technology, Insyringe dSPE, Amine compound

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