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TALANTA · 2017 · IF 4.162

Electrochemically deposited conductive composite sorbent for highly efficient online solid-phase microextraction of jasmonates in plant samples

Xu Ling,Zilin Chen

Conductive composite films composed of poly (3, 4-ethylenedioxythiophene) (PEDOT) and sulfonated graphene were electrochemically deposited on carbon fiber bundle in aqueous solutions for solid phase microextraction (SPME). During the electro-polymerization process, negatively charged sulfonated graphene were doped in PEDOT layer and uniformly dispersed in the composite. The modified carbon fiber bundle worked as sorbent was then successfully applied to online SPME-HPLC-UV analysis of jasmonates in wintersweet flowers. High extraction efficiency (over 420-fold), low limits of detection (0.1   ng   mL −1 for jasmonic acid and 0.01   ng   mL −1 for methyl jasmonate) and wide linear ranges (0.5–5000 and 0.05–5000   ng   mL −1 , R>0.9997) have been obtained. It has been demonstrated that this method can be well used for jasmonates analysis in fresh wintersweet flowers with good recoveries (92.4–98.9%). The results were confirmed by HPLC-MS method.

研究领域: 分析化学 · 植物学
✓ 已验证 DOI PubMed 高影响因子
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ANALYTICAL CHEMISTRY · 2016 · IF 5.886

Efficient and Selective Enrichment of Ultratrace Cytokinins in Plant Samples by Magnetic Perhydroxy-Cucurbit[8]uril Microspheres

Qianchun Zhang,Gongke Li,Xiaohua Xiao,Song Zhan,Yujuan Cao

Cytokinins play a critical role in controlling plant growth and development, but it is difficult to be determined in plant samples due to the extremely low concentration level of picomole/gram. So it is important for efficient sample preparation with selective enrichment and rapid separation for accurate analysis of cytokinins. Herein, a supramolecular perhydroxy-cucurbit[8]uril (PCB[8]) was fabricated into the Fe3O4 magnetic particles via chemical bonding assembly and magnetic perhydroxy-cucurbit[8]uril (MPC) materials were obtained. The MPC had good enrichment capability to cytokinins and the enrichment factors were more than 208. The interaction of MPC and cytokinins was investigated by adsorption test and density functional theory (DFT) calculation, the results showed that the main drive forces were the host–guest interaction and hydrogen-bonding interaction between the perhydroxy-cucurbit[8]uril with analytes. Combined with ultra performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS), the MPC was used as a sorbent of magnetic solid-phase extraction for the analysis of cytokinins in plant samples. A sensitive and selective UPLC–MS/MS method was developed with low detection limits of 0.14–0.32 ng/L for cytokinins analysis. Five cytokinins including zeatin riboside, meta-topolin, kinetin, kinetin riboside, and zip with 6.12–87.3 ng/kg were determined in the soybean sprout and Arabidopsis thaliana. The recoveries were in the range of 76.2–110% with relative standard deviations (n = 5) of 2.3–9.7%. On the basis of these results, magnetic perhydroxy-cucurbit[8]uril materials with selective enrichment capability have good potential on the analysis of ultratrace targets from complicated sample matrixes.

研究领域: 植物学 · 分析化学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

A high-performance light-driven photoelectrochemical sensor based on CdIn2S4/b-TiO2/GO type-II 2D/3D heterojunction for the detection of baicalein in natural plant samples

Xiaoqian Sun,Rongjie Li,Yilin Wang,Kaijia Liu,Yuhui Qiu,Kunxiang Deng,Yixi Xie,Pengcheng Zhao,Junjie Fei

The remarkable pharmacological activities of flavonoids and their effects on human health have prompted many studies. To solve the problem that flavonoids are difficult to be accurately quantified, a novel photoelectrochemical (PEC) sensor based on CdIn 2 S 4 /b-TiO 2 /GO was created to detect the baicalein (BCA). By using physical ultrasonic compounding, a straightforward and effective CdIn 2 S 4 /b-TiO 2 /GO composite was created. The composite’s photoelectric effect was 14 times greater than that of the individual material. When BCA was present, a flavonoid-TiO 2 nanoconjugate was formed based on the interaction between b-TiO 2 and BCA. This interaction prevented the formation and decreased charge transfer of photoporous holes, resulting in a significant decline in photocurrent. Therefore, the PEC sensor based on the change of the electrode surface state can realize the sensitive detection of BCA. The PEC sensor has a wide linear detection range of 1 nM − 30 μM with a limit of detection of 0.5 nM. In addition, the sensor has exhibited excellent accuracy in detecting BCA in the roots and leaves of Scutellaria baicalensis, which can be used for the detection of actual samples.

研究领域: 药理学 · 分析化学 · 材料科学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2020 · IF 4.192

Rapid Analysis of Monosaccharides in Sub-milligram Plant Samples Using Liquid Chromatography–Mass Spectrometry Assisted by Post-column Derivatization

Sha Li,Wen-Jing Cai,Wei Wang,Meng-Xiang Sun,Yu-Qi Feng

Monosaccharides play important roles in plant growth and development, and their biofunctions are closely related to their endogenous contents. Therefore, the determination of monosaccharides is beneficial for the further study of monosaccharide biofunction. In this work, we developed a liquid chromatography–mass spectrometry analytical method assisted by a post-column derivatization technique (LC–PCD–MS) for the fast and automatic determination of 16 monosaccharides in samples. Post-column chemical derivatization of monosaccharides was performed by a reaction of monosaccharides with 4-benzylaminobenzeneboronic acid (4-PAMBA) through boronate ester formation in a three-way connector. 4-PAMBA worked as a derivatization reagent to improve the selectivity and sensitivity of monosaccharide detection by MS. The developed LC–PCD–MS method integrates LC separation, chemical derivatization, and MS detection in one run, thus greatly reducing the analysis time for each sample. The limits of detection and limits of quantification for 16 monosaccharides were in the range of 0.002–0.1 and 0.007–0.5 ng/mL, respectively. Good linearity was obtained from the linear regression, with a determination coefficient (R2) ranging from 0.9928 to 1.0000. The relative recoveries were in the range of 80.7–117.8%, with the intra- and interday relative standard deviations less than 19.7 and 16.5%, respectively, indicating good accuracy and acceptable reproducibility of the method. Finally, the method was successfully applied to investigate the spatial and temporal distribution of 16 monosaccharides in the developing flower and germinating seed of Arabidopsis thaliana.

CAS / MDL: 25895-60-7
研究领域: 植物学 · 分析化学
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ANALYST · 2014 ·Vol. 139 ·期 13 ·3446-3454 · IF 3.906

Isotope labelling – paired homologous double neutral loss scan-mass spectrometry for profiling of metabolites with a carboxyl group

Yun-Qing Huang,Qiu-Yi Wang,Jia-Qi Liu,Yan-Hong Hao,Bi-Feng Yuan,Yu-Qi Feng

We developed a novel method for non-targeted screening of metabolites by high performance liquid chromatography-mass spectrometry with paired homologous double neutral loss scan mode after in vitro isotope labelling (IL-HPLC-PHDNL-MS). As a proof of concept, we investigated the carboxylic acid metabolite profiling in plant samples by the IL-HPLC-PHDNL-MS method. To this end, N,N-dimethylaminobutylamine (DMBA) and d4-N,N-dimethylaminobutylamine (d4-DMBA) were synthesized and utilized to label carboxylic acids. Our results show the MS response of carboxylic acids was enhanced by 20- to 40-fold after labelling. As for the IL-HPLC-PHDNL-MS analysis, DMBA and d4-DMBA labelled samples were mixed equally before MS analysis. Because the isotope labelled moieties (dimethylamino moiety, Me2N) of DMBA and d4-DMBA are easily ruptured and lost as neutral fragments (NL 45 and NL 49) under collision induced dissociation (CID), two neutral loss scans can be carried out simultaneously to record the signals of DMBA and d4-DMBA labelled samples, respectively. In this respect, the metabolites from two samples labelled with different isotope reagents are ionized at the same time but recorded separately by mass spectrometry, which can eliminate the MS response fluctuation and mutual interference. Using this method, six potential biomarkers involved in wounded tomato leaves were identified, and their structures were further elucidated by product ion scan and high resolution mass spectrometry analysis. Taken together, the IL-HPLC-PHDNL-MS method demonstrated good performance on the identification as well as relative quantification of metabolites with a carboxyl group in biological samples.

研究领域: 分析化学 · 代谢组学
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ANALYTICAL CHEMISTRY · 2017 · IF 6.32

Spatial Profiling of Gibberellins in a Single Leaf Based on Microscale Matrix Solid-Phase Dispersion and Precolumn Derivatization Coupled with Ultraperformance Liquid Chromatography-Tandem Mass Spectrometry

Ting Deng,Dapeng Wu,Chunfeng Duan,Xiaohui Yan,Yan Du,Jun Zou,Yafeng Guan

A spatial-resolved analysis method for profiling of gibberellins (GAs) in a single leaf was developed on the basis of microscale sample preparation and precolumn derivatization coupled with ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The proposed microscale sample preparation was based on modified matrix solid-phase dispersion (MSPD) method, in which the plant sample (<1 mg) and C18 sorbent were ground together in one microcentrifuge tube, and then extraction solvent was added followed by centrifugation. In this protocol, the grinding, extraction, and purification were performed in one microcentrifuge tube without any sample transfer step, resulting in an obvious decrease in sample loss. Moreover, a new derivatization reagent, 3-bromopropyltrimethylammonium bromide (BPTAB), was used to further enhance the signal intensities of GAs on MS by 3–4 orders of magnitude, which was much higher than the reported derivatization reagents for GAs such as bromocholine bromide and 3-bromoactonyltrimethylammonium bromide. The present method showed high sensitivity (minimum detectable amount (MDA) of 10.1–72.3 amol for eight GAs) and low sample consumption (down to 0.30 mg FW). Under the optimized conditions, the distribution of GA19 in a single Arabidopsis thaliana leaf was profiled with a spatial resolution of 2 × 2 mm2.

CAS / MDL: 541-46-8
研究领域: 植物学 · 分析化学
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