Analytical Methods
·
2014
·Vol. 6
·期 18
·7518-7524
·
IF 1.938
Nengsheng Ye,Ting Gao,Jian Li
Molecularly imprinted polymers (MIPs) of dopamine (DA) were constructed on the surface of graphene oxide (GO), and attached inside the pores of hollow fibers (HFs) for the solid-phase microextraction (SPME) of DA. Scanning electron microscopy, thermogravimetric analysis and Raman spectroscopy indicated that GO–MIP composites were successfully synthesized and modified in the pores of HFs via ultrasonication. Compared with common HFs and HFs modified with non-imprinted polymers (GO–NIP/HF) using the same SPME procedures, the GO–MIP/HF composites showed the best efficiency for the extraction of DA. The selectivity of GO–MIP/HF was investigated based on the selectivity factor (F) using epinephrine and norepinephrine as the structural analogues of DA. The linear range of dopamine was 1.05 × 10−3 to 5.27 × 10−3 μmol mL−1, using this process with a detection limit of 2.64 × 10−4 μmol mL−1. The extraction procedure based on GO–MIP/HF was successfully used for the determination of DA in human serum and its hydrochloride injection, showing average recoveries of 83–96%. GO–MIP/HF was a good carrier for the selective adsorption of DA, and showed promise for the preconcentration of DA in real samples.
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CHROMATOGRAPHIA
·
2013
·Vol. 76
·期 23
·1641-1647
·
IF 1.437
Yang Qing,Chen Xiaoqing,Jiang Xinyu
A novel, efficient, and environmentally friendly method—supramolecular solvent liquid–liquid microextraction (SMS-LLME) combined with high-performance liquid chromatography (HPLC)—was first established for the determination of p -nitrophenol and o -nitrophenol in water samples. Several important parameters influencing extraction efficiency, such as the type and volume of extraction solvent, pH of sample, temperature, salt effect, extraction time, and stirring rate, were optimized in detail. Under the optimal conditions, the enrichment factor was 166 for p -nitrophenol and 160 for o -nitrophenol, and the limits of detection by HPLC were 0.26 and 0.58 μg L −1 , respectively. Excellent linearity with coefficients of correlation from 0.9996 to 0.9997 was observed in the concentration range of 2–1,000 μg L −1 . The ranges of intra- and interday precision ( n = 5) at 100 μg L −1 of nitrophenols were 5.85–7.76 and 10.2–11.9 %, respectively. The SMS-LLME method was successfully applied for preconcentration of nitrophenols in environmental water samples.
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ANALYST
·
2015
·Vol. 141
·期 3
·1083-1090
·
IF 4.107
Yi Zhang,Yan Zhang,Guan Wang,Wujuan Chen,Pingang He,Qingjiang Wang
A novel Congo red (CR) derivatized silica stationary phase was prepared and packed into a fused silica capillary tube for nano-flow HPLC. A variety of analytes including poly-aromatic hydrocarbons, parabens, acids, sulfonamides, bases, and nucleosides were successfully separated using the CR. In comparison with commercial ODS columns, this new stationary phase has a different separation mechanism (hydrophobically-assisted ion-exchange), which was evident in the separation of benzoic acid derivatives and sulfonamides. The successful application of CR-bonded silica stationary phase in the HILIC and PALC modes demonstrates the effectiveness of this potential chromatographic material in nano flow HPLC.
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MICROCHIMICA ACTA
·
2015
·Vol. 183
·期 2
·589-596
·
IF 3.741
Tang Yiwei,Li Min,Gao Xue,Liu Xiuying,Ma Yong,Li Yi,Xu Yongxia,Li Jianrong
Hollow molecularly imprinted polymers (h-MIPs) consisting of K 2 Ti 4 O 9 as a sacrifice matrix were synthesized for selective recognition of enrofloxacin (ENR). The h-MIPs possess a characteristic nanostructure and were characterized by Fourier transform infrared spectroscopy, X-ray powder diffraction and transmission electron microscopy. The h-MIPs have a fast adsorption kinetic (~10 min), high adsorption capacity and a good selectivity factor (2.4) for ENR. Following adsorption of ENR, it was eluted from the sorbent with methanol-acetic acid (8:2) and quantified by HPLC. The calibration plot extends from 0.5 to 16.0 ng mL‾ 1 of ENR with a correlation coefficient of 0.9912, and the limit of detection is 0.24 ng mL‾ 1 (at an S/N ratio of 3). The method was applied to the determination of ENR in spiked fish samples, and recoveries ranged from 68.88 to 100.29 % with relative standard deviations (for n = 3) between 1.6 and 4.4 %.
Hollow molecularly imprinted polymers (h-MIPs) were synthesized using K 2 Ti 4 O 9 as sacrifice matrix for selective recognition of enrofloxacin (ENR). These MIPs served as an SPE adsorbent for purification and enrichment of ENR prior to quantitation by HPLC
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MOLECULES
·
2024
·Vol. 29
·期 11
·2560
·
IF 4.2
Qundong Liu,Huanhuan Yu,Yuzhuo Dong,Wenjing Quan,Zhimin Su,Longyun Li
Lonicera macranthoides, the main source of traditional Chinese medicine Lonicerae Flos, is extensively cultivated in Southwest China. However, the quality ofL. macranthoidesproduced in this region significantly varies due to its wide distribution and various cultivation breeds. Herein, 50 Lonicerae Flos samples derived from different breeds ofL. macranthoidescultivated in Southwest China were collected for quality evaluation. Six organic acids and three saponin compounds were quantitatively analyzed using HPLC. Furthermore, the antioxidant activity of a portion of samples was conducted with 2,2′-Azinobis-(3-ethylbenzthiazoline-6-sulphonate) (ABTS) and 1,1-diphenyl-2-picryl-hydrazyl (DPPH) radical scavenging experiments. According to the quantitative results, all samples met the quality standards outlined in the Chinese Pharmacopoeia. The samples from Guizhou, whether derived from unopened or open wild-type breeds, exhibited high quality, while the wild-type samples showed relatively significant fluctuation in quality. The samples from Chongqing and Hunan demonstrated similar quality, whereas those from Sichuan exhibited relatively lower quality. These samples demonstrated significant abilities in clearing ABTS and DPPH radicals. The relationship between HPLC chromatograms and antioxidant activity, as elucidated by multivariate analysis, indicated that chlorogenic acid, isochlorogenic acid A, isochlorogenic acid B, and isochlorogenic acid C are active components and can serve as Q-markers for quality evaluation.
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EUROPEAN JOURNAL OF MEDICINAL CHEMISTRY
·
2024
·
IF 6
Qingqing Zhang,Yuying Liu,Jie Zhang,Yanchen Li,Jin Wang,Nanxin Liu,Jie Zhang,Xiaoyan Pan
Proteolysis targeting chimeras (PROTAC) are bifunctional chimeric molecules capable of directly degrading binding proteins through the ubiquitin-proteasome pathway. PROTACs have demonstrated significant potential in overcoming drug resistance and targeting previously untreatable targets. However, several limitations still need to be addressed, including their high molecular weight resulting in poor membrane permeability and bioavailability. In this study, we proposed that cancer-targeted penetrating peptides could enhance the cell permeability of PROTACs. We developed 26 novel targeted penetrating peptides for leukemia and lymphoma cells, among which C9C-f(3Bta) and Cyclo-C9C–R exhibited superior membrane permeability, targetability, and stability. By combining C9C-f(3Bta) and Cyclo-C9C–R with IMA-PROTAC, we effectively enhanced the anti-proliferative activity of IMA-PROTAC, facilitated degradation of Bcr-Abl protein in K562 cells, and reduced downstream STAT5 phosphorylation. Furthermore, the combined application promoted cell apoptosis while blocking G1 phase progression. HPLC-MRM-MS revealed that the combination of C9C-f(3Bta) or Cyclo-C9C–R with IMA-PROTAC significantly enhanced intracellular IMA-PROTAC content. In summary, our proof-of-concept study validated the hypothesis that combining PROTACs with targeted penetrating peptides can improve protein degradation efficiency as well as anti-proliferative capabilities.
研究领域:
肿瘤学
·
药理学
·
分子生物学
·
细胞生物学
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Wenwen Wang,Yun Shi,Yiwen Tian,Chenlu Liu,Nuo Xu,Chunhui Liu,Chenfeng Zhang,Jie Yang,Kunming Qin,Qing Zhang
A comprehensive assessment of the total flavonoid content and antioxidant activities of 13 medicinal materials was conducted utilizing high-performance liquid chromatography with ultraviolet-visible detector (HPLC-UVD) and spectral-effect relationship analysis. The contents of seven flavonoids were quantified, and chemometric methods including hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) were applied to differentiate the samples. One-way analysis of variance (ANOVA) identified specific herbs for which both flavonoid profiles and antioxidant capacity varied significantly with geographical origin, underscoring the impact of provenance on bioactive quality. The results revealed significant variations in flavonoid composition, with isoquercitrin, quercetin, kaempferol, isorhamnetin, and hyperoside being identified as the key contributors to quality. A structure-activity relationship analysis was employed to elucidate how specific molecular features, such as hydroxylation and glycosylation patterns, influenced antioxidant efficacy. In vitro antioxidant assays (2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2’-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical scavenging) ranked Houttuyniae Herba as the most potent, followed by Rubi Fructus and Albiziae Flos . Grey relational analysis (GRA) identified isoquercitrin, astragalin, and hyperoside as the primary flavonoids correlated with antioxidant capacity. This work provides a scientific basis for quality assessment and bioactive component screening in multi-source medicinal materials.
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2018
·
IF 0.827
Huihui Wu,Hanying Jin,Guangxin Yuan,Jacques Crommen,Jing Zhang,Qiqin Wang
Urea and allantoin are two important additives in cosmetic products for the treatment of dry skin as well as for skin protection and regeneration. In this research, a highly hydrophilic monolith prepared by co-polymerization of N,N-dimethyl-N-acryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPDA) and N,N’-methylenebisacrylamide (MBA) was first exploited for the simultaneous quantification of urea and allantoin in cosmetic products by nano-HPLC in the HILIC mode. The whole separation process could be completed within six minutes using isocratic elution. Due to the extremely high hydrophilicity of this monolithic column, a relatively low content (80%) of ACN in the mobile phase was required to achieve satisfactory separation, and therefore the solubility problems for polar compounds was also avoided in comparison with previously reported results on the commercial columns. Method validation was also accomplished with respect to linearity, reproducibility, selectivity, recovery, stability, LOD and LOQ. The recoveries of urea and allantoin from spiked cosmetic samples were 95.6%-100% and 94.1%-99.9%, respectively. Validation results indicate that this HILIC method based on the miniaturized poly(SPDA-co-MBA) monolith can be applied successfully to the fast and efficient determination of urea and allantoin in cosmetic samples. The miniaturized column format, the low sample consumption (20 nL), and excellent separation efficiency could make this highly hydrophilic monolith an attractive choice for the detection of trace polar analytes from complex samples in future.
研究领域:
分析化学
·
化妆品科学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Ting-ting Du,Ting Cui,Hong-mei Qiu,Nian-ru Wang,Dan Huang,Xin-hui Jiang
A high-performance liquid chromatography method with a diode array and an electrochemical detection (HPLC-ECD/DAD) was developed to determine the levels of tryptophan (TRP), kynurenine (KYN), kynurenic acid (KYA), 5-hydroxytryptamine (5-HT) and 5-hydroxyindoleacetic acid (5-HIAA) in rat plasma. The prepared samples were separated on a BDS column (4.6 mm × 250 mm, 5 mm) with column oven temperature of 25 °C. The mobile phase consisted of 5% acetonitrile and a buffer solution, which contained 25 mmol/L sodium acetate and 0.01 mmol/L EDTA, adjusting pH to 4.5 with acetic acid, and it was pumped at a flow-rate of 1.0 mL/min. KYN and KYA were measured by a variable wavelength detector at wavelengths 360 nm and 333 nm respectively, TRP and vanillic acid (as IS) both were measured at 280 nm. Determination of 5-HT and 5-HIAA was accomplished at the electrochemical working potential of 700 mV. Total run time was 14 min. Several parameters of the developed method were validated including linearity, accuracy precision, and stability. The results showed the established method had good LOD and separation for all of the five compounds and IS in the biological matrix. The method is simple, fast, economical and accurate. The analytical method and the results could provide a reference for the clinical and scientific research of depression.
研究领域:
分析化学
·
神经科学
·
药理学
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Journal of Food Measurement and Characterization
·
2026
·
IF 3.6
Puah Boon-Peng,Jalil Juriyati,Attiq Ali,Kamisah Yusof,Jamal Jamia Azdina
Dragon fruit ( Hylocereus spp.) is widely cultivated in Southeast Asia and is known for its nutritional and medicinal properties. Despite this potential, dragon fruit peel remains an underutilized by-product, while previous studies have largely focused on antioxidant activity, membrane-stabilizing effects, or enzyme-based anti-inflammatory assays, with limited evidence on cytokine modulation in human macrophages. Therefore, this study aimed to evaluate the anti-inflammatory activity of crude extracts and solvent-partitioned fractions from Hylocereus costaricensis (red flesh) and H. undatus (white flesh), and to characterize the phytochemical profiles of the most active fractions. Crude extracts were prepared using 80% ethanol and subsequently fractionated with hexane, ethyl acetate, and butanol. Cytotoxicity was assessed in phorbol 12-myristate 13-acetate (PMA)-differentiated THP-1 human macrophages using the methyl thiazolyl tetrazolium (MTT) assay, while anti-inflammatory activity was evaluated in lipopolysaccharide (LPS)-stimulated THP-1 macrophages by quantifying interleukin-1 beta (IL-1β), interleukin-6 (IL-6), and tumor necrosis factor alpha (TNF-α). All samples demonstrated low cytotoxicity up to 500 µg/mL. The peel hexane fractions showed the most pronounced cytokine suppression, particularly against IL-1β (81–84%) and IL-6 (74–75%), whereas TNF-α inhibition was moderate. Concentration–response studies revealed that the H. undatus peel hexane fraction was the most potent with IC 50 of 5.73 µg/mL and 76.64 µg/mL for IL-1β and IL-6, respectively. High-performance liquid chromatography (HPLC) identified β-amyrin and campesterol in both active fractions, while gas chromatography–mass spectrometry (GC-MS) detected fatty acids, tocopherols, and triterpenoids. Although H. costaricensis peel contained higher levels of β-amyrin (0.59%) and campesterol (2.83%), H. undatus peel (0.15% β-amyrin; 1.86% campesterol) showed stronger cytokine inhibition, suggesting that multiple lipophilic constituents may contribute to the observed activity. These findings indicate that dragon fruit peel lipophilic fractions are promising sources of cytokine-suppressive constituents and provide analytical support for the valorization of this underutilized by-product as functional food or nutraceutical ingredients.
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MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Huizhen Zhao,Hui Li,Wenhui Lu,Shanchao Fu,Deyi Zhu,Shan Cao,Lingxin Chen,Jinhua Li
High concentration of surfactant, lipid, metal salts, tanning agent, dye and other leather auxiliaries contain in wet-blue, crust leather and tannery wastewater. The existence of these complicated matrices seriously affects the performance of analytical instruments and the accuracy of conventional analytical methods. In this study, to effectively avoid matrix interference of leather and tannery wastewater by simple pretreatment process, thermo-magnetic dual-template molecularly imprinted polymers (TM-dt-MIPs) were prepared and used as magnetic solid-phase extraction (MSPE) adsorbent to simultaneously selective extract ten kinds of phenols (phenol, five chlorophenols (CPs), and four alkylphenols (APs)), coupled with HPLC analysis. The TM-dt-MIPs prepared by stimuli-responsive imprinting and multi-template imprinting techniques utilized magnetic graphene oxide-multiwalled carbon nanotubes as supporting material, N-isopropyl acrylamide and methacrylamide as functional monomers, 2,4-dichlorophenol and nonylphenol as dual template, showing uniform morphology, high magnetic property and thermal stability. Crucially, the thermo-sensitivity and adsorption ability for target phenols were assessed through thermo-regulated capture/release, static, dynamic and selective adsorption studies, confirmed that the adsorption and desorption of the target analytes could be effectively controlled by external temperature regulation and magnetic manipulation. The developed TM-dt-MIPs-MSPE-HPLC method exhibited excellent analytical performance, characterized by high enrichment factors (26.63–110.4), wide linear ranges (2–200 μg L −1 ), low limits of detection (0.10–0.36 μg L −1 ), limits of quantitation (0.34–1.21 μg L −1 ) and good precision (intra-day RSD: 1.61–6.84%; inter-day RSD: 2.15–8.51%). For the analysis of ten phenols in crust leather, wet blue, and tannery wastewater samples, satisfactory recoveries were achieved ranging from 72.27 to 119.6%, demonstrating the practical application prospects for trace phenol analysis in leather industrial matrices.
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MOLECULES
·
2026
·Vol. 31
·期 6
·
IF 5.1
Jichao Liu,Xiuzhuang Li,Jiaojiao Yu
Fluoroquinolones (FQs) are a kind of antibiotics, which are widely used in animal husbandry and aquaculture. However, the abuse of FQs can result in residues in foodstuffs of animal origin. Therefore, it is essential to establish a sensitive and accurate detection method for determination of FQs in food samples. An effective sample pretreatment method is a crucial procedure for enrichment of trace target compounds from complex matrix before HPLC analysis. As an emerging kind of sample pretreatment methods, magnetic solid-phase extraction (MSPE) has attracted much interest due to its characteristics including low cost, simplicity, and rapidity. In this study, a novel fluorinated magnetic covalent organic framework (Fe3O4@PDA@COF) was fabricated, which was used as an adsorbent in MSPE as well as coupled with HPLC to determine FQs in food samples. Under optimal conditions, the developed Fe3O4@PDA@COF-MSPE-HPLC-UV method possessed a wide linear range (1–250 µg·kg−1) and low limits of detection (0.5–0.7 µg·kg−1) with good linearity (R2≥ 0.9938). Additionally, the method has been used to adsorb FQs from chicken samples. The recoveries of target FQs in spiked samples were 84.2–106.7% with relative standard deviations (RSDs) below 7.8%. These results demonstrated that the established method provides an efficient and sensitive solution for monitoring FQ residues in foodstuffs.
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