Layer-by-layer functionalized porous Zinc sulfide nanospheres-based solid-phase extraction combined with liquid chromatography time-of-flight/mass and gas chromatography-mass spectrometry for the specific enrichment and identification of alkaloids from Cr

Layer-by-layer functionalized porous Zinc sulfide nanospheres-based solid-phase extraction combined with liquid chromatography time-of-flight/mass and gas chromatography-mass spectrometry for the specific enrichment and identification of alkaloids from Cr
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基于层层功能化多孔硫化锌纳米球的固相萃取结合液相色谱-飞行时间/质量和气相色谱-质谱联用技术对Cr中的生物碱进行特异性富集和鉴定

DOI:
10.1016/j.aca.2016.05.028
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发表时间:
2016-08
影响因子:
6.2
通讯作者:
Hu Yue
Hu Yue
中科院分区:
化学1区
文献类型:
--
作者:
Zhu Dong;Miao Zhao Yi;Yang Rui Xiang;Wen Hong Mei;Li Wei;Chen Jun;Kang An;Shan Chen-Xiao;Yu Sheng;Hu Yue

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目前广泛使用的聚合物或C8、C18封端材料基固相萃取吸附剂仅基于“同类相溶”原理不能很好地捕获生物碱。本文建立了一种基于硫化锌纳米球的固相萃取-液相色谱-飞行时间质谱(LC-TOF/MS)和气相色谱-质谱(GC-MS)联用技术,用于复杂基质--中华卷叶草粗提物中生物碱的特异性富集和鉴定。通过聚丙烯酸(PAA)均聚物与ZnS纳米球的酰胺化反应,制备了功能化多孔ZnS纳米球。LC-TOF/MS联用分析表明,固相萃取洗脱液中的23个主要峰几乎全部为生物碱类化合物,根据氮原子规则和峰命中率公式,结合色谱保留指数,确定了7个生物碱类化合物,其中包括2个新发现的化学实体。我们相信,这种SPE协议也可以在未来利用选择性地富集生物碱从其他植物物种的提取物。
The current widely utilized polymer or C8, C18 end-capped material-based sorbents for solid-phase extraction could not capture alkaloids well only based on “like dissolves like” principle. In this paper, a layer-by-layer functionalized porous Zinc sulfide nanospheres-based solid-phase extraction (SPE) combined with liquid chromatography time-of-flight/mass spectrometry (LC-TOF/MS) and gas chromatography-mass spectrometry (GC-MS) was developed for the specific enrichment and identification of alkaloids from complex matrixes,Crinumasiaticumvar.sinicumcrude extracts. The functionalized porous Zinc sulfide nanospheres were prepared by the amidation reaction of poly-(acrylic acid) (PAA) homopolymer with amino groups onto the porous ZnS nanospheres. Tandem LC-TOF/MS spectrometry presented that the almost all of the twenty-three main peaks in elution fraction from the SPE could be inferred as alkaloids with ion of mass according to the nitrogen rule and hit formula with Peak View1.2@software from AB SCIEX, and seven alkaloids including two new found chemical entities were directly identified from their GC-MS spectra and retention indices. We believe that this SPE protocol can also be utilized in the future to selectively enrich alkaloids from extracts of other plant species.
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