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TALANTA · 2022 · IF 6.556

A guide of column selection for two-dimensional liquid chromatography method development of natural alkaloids

Yang Xu,Yanfang Liu,Han Zhou,Rong Wang,Dongping Yu,Zhimou Guo,Xinmiao Liang

Natural products , especially alkaloids, are one of the most valuable, potential drug leads in drug discovery. As an efficient tool for complex samples, two-dimensional liquid chromatography (2D-LC) has become a powerful means of analysis and separation of natural alkaloids. Method development of 2D-LC is of great importance because it helps to enhance the selectivity, resolution and peak capacity of a separation system. However, due to the diversity of the nature and subclasses of natural alkaloids, peak tailing occurs frequently, making alkaloid separation complicated and time-consuming. To conquer such difficulties, we proposed a guide for column selection and combination in 2D-LC so as to improve the alkaloid separation. Based on a comprehensive evaluation of applicability and orthogonality of several columns, this guide would provide a simple but clear starting point for column selection of 2D-LC method development. The evaluation included seven columns to involve most separation mechanisms reported in alkaloid separation, and 49 natural alkaloid standards of various subclasses and natures. Detailed studies of peak shapes of every column were carried out as well, providing useful references to better understand the peak tailing issues of some analytes on specific columns. Subsequently, a 2D-LC method was developed using our guide to isolate an alkaloid sample from U. rhynchophylla , generating symmetrical peaks and a high orthogonality of 80.3%. Further, this evaluation process would help to have a quick understanding when a new stationary phase is designed.

CAS / MDL: 540-69-2 64-18-6
研究领域: 分析化学 · 药学 · 天然产物化学
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TALANTA · 2023 · IF 6.1

Multicolor aptasensors for pesticide multiresidues detection in agricultural products using bioorthogonal surface-enhanced Raman scattering tags

Mengmeng Yan,Hao Wang,Min Li,Wenjun Zhang,Hongxia Du,Zilei Chen,Chao Zhu,Yongxin She

Realizing accurate pesticide multiresidue detection in a complex matrix is still a challenge for point-of-care sensing methods. Herein, we introduced background-free and multicolor aptasensors based on bioorthogonal surface-enhanced Raman scattering (SERS) tags and successfully applied them to analyze multiple pesticide residues . The excellent anti-interference and multiplex capability are due to the application of three bioorthogonal Raman reporters involving 4-ethenylbenzenamine (4-EBZM), Prussian blue (PB) and 2-amino-4-cyanopyridine (AMCP) with alkynyl and cyano groups , which demonstrated apparent Raman shift peaks at 1993 cm −1 , 2160 cm −1 , and 2264 cm −1 in the biologically Raman-silent region, respectively. Ultimately, a detection range of 1–50 nM for acetamiprid , atrazine and malathion was achieved with detection limits of 0.39, 0.57 and 0.16 nM, respectively. The developed aptasensors were successfully used to determine pesticide residues in real samples. These proposed multicolor aptasensors offer an effective strategy for pesticide multiresidue detection with advantages of anti-interference, high specificity and high sensitivity.

研究领域: 分析化学 · 食品安全 · 环境科学
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Separation Science Plus · 2023 · IF 1.1

Preparation of polyvinyl pyrrolidone stationary phase and its application in separation and analysis of flavonoids

Xin Chen,Juntao Li,Mengting Gu,Yiyuan Miao,Yanxiong Ke,Xiangwei Zheng,Jian Xu

Polyvinylpyrrolidone (PVP) is known as a polymer with special adsorption properties for polyphenolic compounds. In this paper, chemical-bonded stationary phase (PVP@Silica) was prepared and applied to the separation of flavonoids. System constants determined by linear solvation energy relationships with methanol–water mixtures as the mobile show that the column can provide stronger hydrogen bonding and π–π interaction than C18 column. Under reversed-phase conditions, traditional flavonoids have much longer retention on PVP@Silica than on C18 column with methanol–water mobile phase due to multimodal retention mechanism, including hydrogen bonding and π–π interaction. In addition, a U-shaped retention curve was observed in acetonitrile–water mobile phase because of the enhanced hydrogen bonding under the high proportion of acetonitrile. The selectivity to polyhydroxy structure gives the stationary phase unique separation ability for flavonoids. The separation orthogonality was further investigated by a sample set containing 33 flavonoids with different substitution structures. The (RP-PVP@Silica)-(RP-C18) system exhibited 60% orthogonality metric (OM) for these flavonoids with methanol–water mobile phase. A high OM of 63.5% was achieved in (RP-PVP@Silica)-(HILIC-PVP@Silica) system. Finally, PVP@Silica was applied to the purification of total flavonoids in Ginkgo biloba extract (GBE). The offline (RP-PVP@Silica)-(RP-C18) two-dimensional separation system was used for the analysis of flavonoids in GBE.

研究领域: 分析化学 · 药学
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CHEMISTRY-A EUROPEAN JOURNAL · 2021 ·Vol. 27 ·期 49 ·12589-12598 · IF 5.236

Infrared Responsive Choline Phosphate Lipids for Synergistic Cancer Therapy

Sangni Jiang,Wenliang Wang,Lihua Dong,Xinxin Yan,Shengran Li,Weikang Mei,Xintao Xie,Yuanhua Zhang,Sanrong Liu,Xifei Yu

Graphical Spot on : A light-inducible Lip-cRGDfk/ICG/Dox liposome simultaneously loads a water-soluble drug (Dox) and photothermal transduction agents (ICG), targets the tumor site, and locally heats it up under external laser irradiation. Due to the conformational transformation of CP lipids, the anticancer drug Dox is released at a specific time and in a specific space to kill tumor cells. This brings about a combination of chemotherapy and photothermal therapy for the noninvasive treatment of tumors. Choline phosphate lipids have been designed and developed as new-generation zwitterionic nanocarriers with excellent biocompatibility and bioorthogonality to provide a more programmable performance for cancer therapy. However, there is a lack of spatiotemporal and reversible control for drug release at target tumor cells, which can lead to severe adverse effects to normal tissue and discounted treatment outcome. Here, light-inducible Lip-cRGDfk/ICG/Dox liposomes were developed for synergistic cancer therapy. ICG can effectively convert light energy into selective heating in a local environment upon laser irradiation, thus inducing thermal ablation of tumor cells, and further reversibly trigger the spatiotemporal release of anticancer drugs (Dox) at tumor cells due to the conformation transformation of CP lipids to synergistically kill tumor cells. That Lip-cRGDfk/ICG/Dox exhibited a significant improvement for breast cancer therapy in vitro and in vivo is also demonstrated, thus it can serve as an efficient platform to noninvasively and spatiotemporally control the activation of cytotoxicity at tumor cells for precision cancer therapy.

研究领域: 癌症治疗 · 纳米技术 · 药学 · 生物医学工程
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