Identification of Efficacy-Associated Markers to Discriminate Flos Chrysanthemum and Flos Chrysanthemi Indici Based on Fingerprint-Activity Relationship Modeling: A Combined Evaluation over Chemical Consistence and Quality Consistence.

Monitoring the quality consistency of traditional Chinese medicines, or herbal medicines (HMs), is the basis of assuring the efficacy and safety of HMs during clinical applications. The purpose of this work was to characterize the difference in hydrophilic antioxidants and related bioactivities between Flos Chrysanthemum (JH) and its wild relatives (Chrysanthemum indicum L.; YJH) based on the establishment of fingerprint-efficacy relationship modeling. The concentrations of the total phenolics and flavonoids of JH samples were shown to be generally higher than those of YJH, but the concentration distribution ranges of YJH were significantly greater compared to JH samples, possibly related to environmental stress factors leading to the concentration fluctuations of phytochemicals during the growth and flowering of Chrysanthemum cultivars. Correspondingly, the total antioxidant capabilities of JH were greatly higher than those of YJH samples, as revealed by chemical assays, including DPPH and ABTS radical scavenging activities and FRAP assays. In addition, cellular-based antioxidant activities confirmed the results of chemical assays, suggesting that the differences in antioxidant activities among the different types of Chrysanthemums were obvious. The extracts from YJH and JH samples showed significant α-glucosidase inhibitory activity and lipase-inhibitory activity, implying the modulatory effects on lipid and glucose metabolisms, which were also confirmed by an untargeted cell-based metabolomics approach. The selected common peaks by similarity analysis contributed to the discrimination of YJH and JH samples, and the modeling of the fingerprint-bioactivity relationship identified neochlorogenic acid, isochlorogenic acid A, and linarin as efficacy-associated chemical markers. These results have demonstrated that integrating HPLC fingerprints and the analysis of similarity indexes coupled with antioxidant activities and enzyme-inhibitory activities provides a rapid and effective approach to monitoring the quality consistency of YJH/JH samples.

Ophiopogon japonicus and its active compounds: A review of potential anticancer effects and underlying mechanisms.

BACKGROUND: Ophiopogon japonicus (Thunb.) Ker Gawl., a well-known Chinese herb, has been used in traditional Chinese medicine for thousands of years. Extensive in vitro and in vivo studies have shown that O. japonicus and its active compounds exhibit potential anticancer effects in a variety of cancer cells in vitro and suppress tumor growth and metastasis without causing serious toxicity in vivo. PURPOSE: This review aims to systemically summarize and discuss the anticancer effects and the underlying mechanisms of O. japonicus extracts and its active compounds. METHODS: The review is prepared following the guidelines of Preferred Reporting Items for Systematic Reviews and Meta-Analyses. Various scientific databases including Web of Science, PubMed, Scopus, and Chinese National Knowledge Infrastructure were searched using the keywords: Ophiopogon japonicus, tumor, cancer, carcinoma, content, pharmacokinetics, and toxicity. RESULTS: O. japonicus extracts and the active compounds, such as ruscogenin-1-O-[ß-d-glucopyranosyl(1→2)][ß-d-xylopyranosyl(1→3)]-ß-d-fucopyranoside (DT-13), ophiopogonin B, and ophiopogonin D, exert potential anticancer effects, including the induction of cell cycle arrest, activation of apoptosis and autophagy, and inhibition of metastasis and angiogenesis. In addition, the mechanisms underlying these effects, as well as the pharmacokinetics, toxicity and clinical utility of O. japonicus extracts and active compounds are discussed. Furthermore, this review highlights the research and application prospects of these compounds in immunotherapy and combination chemotherapy. CONCLUSIONS: The traditional herb O. japonicus and its phytochemicals could be safe and reliable anticancer drug candidates, alone or in combination with chemotherapeutic drugs. We hope that this review, which highlights the anticancer properties of O. japonicus, will contribute to drug optimization, therapeutic development, and future studies on cancer therapies based on this medicinal plant.

Robust boron nanoplatform provokes potent tumoricidal activities via inhibiting heat shock protein.

Near-infrared (NIR)-light-triggered photothermal therapy (PTT) is a promising treatment for breast cancer. However, its therapeutic efficiency is often compromised due to the heat-induced up-regulation of heat shock proteins, which confer photothermal resistance. To solve this urgent problem, PEGylated two-dimensional boron nanosheets (B-PEG)-which allow both multimodal imaging and photothermal conversion-were loaded with gambogic acid (GA), which can inhibit heat shock protein 90 (Hsp90). Experimental findings indicated that this combination of B-PEG and GA could serve as an integrated drug delivery system for cancer diagnosis and treatment. It could be used to administer mild PTT as well as chemotherapy for breast cancer, provide improved anti-tumor effects, and reduce the toxicity of PTT, all while inhibiting breast cancer growth. This drug delivery system could offer a novel tool for administering chemotherapy combined with PTT while avoiding the adverse effects of traditional PTT.

Cell metabolomics study on the anticancer effects of Ophiopogon japonicus against lung cancer cells using UHPLC/Q-TOF-MS analysis.

Ophiopogon japonicus (OJ) is a traditional Chinese herbal medicine that has been used for thousands of years. Recently, the anticancer effects of OJ have been reported in multiple types of cancer, particularly in lung cancer. However, the underlying mechanisms remain unclear. In present study, the effects of OJ against NCI-H1299 human lung cancer cells were investigated, and the underlying mechanisms were explored using ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF-MS)-based cell metabolomics. As a result, OJ inhibited the proliferation, induced the apoptosis and suppressed the migration of NCI-H1299 cells. A total of 22 differential metabolites responsible for the effects of OJ were screened and annotated based on the LC-MS-based cell metabolomics approach. The altered metabolites were involved in three metabolic pathways, including glycerophospholipid metabolism, ether lipid metabolism and glutathione metabolism. These results showed that cell metabolomics-based strategies are promising tools to discover the action mechanisms of OJ against lung cancer cells.

Chemical Comparison of Monk Fruit Products Processed by Different Drying Methods Using High-Performance Thin-Layer Chromatography Combined With Chemometric Analysis.

Monk fruit, also named Luo Han Guo, is the fruit of Siraitia grosvenorii (Swingle) C. Jeffrey ex A. M. Lu et Z. Y. Zhang and has been used as both food and traditional Chinese medicine. Due to preservation concerns, monk fruit is usually processed by hot-air drying or using low-temperature techniques after harvest. In this study, high-performance thin-layer chromatography (HPTLC) method was developed for the analysis of 13 mogrosides, 1 flavonoid, and 3 sugars in monk fruit products. Then chemometric analysis was applied to investigate the chemical characteristics in the samples dried by different methods. The results showed that the contents of mogroside V, 11-oxo-mogroside V, isomogroside V, and sucrose in monk fruits dried at low temperature were much higher than those in traditional hot-air drying samples, which was also confirmed by HPTLC-scanning. These findings indicate that HPTLC combined with chemometric analysis provides a reliable tool to understand the chemical differences between the monk fruit products processed by different drying methods, which will be helpful for their quality evaluation.

Rapid Screening of Lipase Inhibitors from Ophiopogonis Radix Using High-Performance Thin Layer Chromatography by Two Step Gradient Elution Combined with Bioautographic Method.

In this study, a high-performance thin layer chromatography (HPTLC) method by two step gradient elution with two mobile phases was developed for the simultaneous analysis of seven constituents in Ophiopogonis Radix. The chromatography was performed on silica gel 60 F254 plate with dichloromethane-methanol-ethyl acetate-water (70:25:12:3, v/v/v/v) and dichloromethane-methanol (300:1, v/v) as the mobile phase for two step gradient elution. Then, the HPTLC profiles were observed after derivatization with 10% sulfuric acid in ethanol solution. The obtained HPTLC images were further analyzed by chemometric approaches and the samples could be clustered based on regions and/or growth years, which were two important factors affecting the constituents in Ophiopogonis Radix. Furthermore, five compounds including ophiopogonin D, ophiopojaponin C, ophiopogonin D', ophiopogonin C' and methylophiopogonanone B were screened as potential lipase inhibitors from Ophiopogonis Radix by the HPTLC-bioautographic method. The binding modes and interactions between the five compounds and lipase were further explored by molecular docking analysis. The developed HPTLC method could be used for quality control of Ophiopogonis Radix and screening of the potential lipase inhibitors.

Rational Design of Thermosensitive Hydrogel to Deliver Nanocrystals with Intranasal Administration for Brain Targeting in Parkinson's Disease.

Mitochondrial dysfunction is commonly detected in individuals suffering from Parkinson's disease (PD), presenting within the form of excessive reactive oxygen species (ROS) generation as well as energy metabolism. Overcoming this dysfunction within brain tissues is an effective approach to treat PD, while unluckily, the blood-brain barrier (BBB) substantially impedes intracerebral drug delivery. In an effort to improve the delivery of efficacious therapeutic drugs to the brain, a drug delivery platform hydrogel (MAG-NCs@Gel) was designed by complexing magnolol (MAG)-nanocrystals (MAG-NCs) into the noninvasive thermosensitive poly(N-isopropylacrylamide) (PNIPAM) with self-gelation. The as-prepared MAG-NCs@Gel exhibited obvious improvements in drug solubility, the duration of residence with the nasal cavity, and the efficiency of brain targeting, respectively. Above all, continuous intranasal MAG-NCs@Gel delivery enabled MAG to cross the BBB and enter dopaminergic neurons, thereby effectively alleviating the symptoms of MPTP-induced PD. Taking advantage of the lower critical solution temperature (LCST) behavior of this delivery platform increases its viscoelasticity in nasal cavity, thus improving the efficiency of MAG-NCs transit across the BBB. As such, MAG-NCs@Gel represented an effective delivery platform capable of normalizing ROS and adenosine triphosphate (ATP) in the mitochondria of dopaminergic neurons, consequently reversing the mitochondrial dysfunction and enhancing the behavioral skills of PD mice without adversely affecting normal tissues.

Amine modified graphene as reversed-dispersive solid phase extraction materials combined with liquid chromatography-tandem mass spectrometry for pesticide multi-residue analysis in oil crops.

Amine modified graphene is successfully synthesized via a one-pot solvothermal reaction between graphene oxide and ammonia water, methylamine or n-butyl amine. The presence of amine groups in graphene is identified by Fourier-transform infrared spectrometry, X-ray photoelectron spectroscopy and an X-ray diffractometer. The ability of amine modified graphene to cleanup fatty acids and other interfering substances from acetonitrile extracts of oil crops has been evaluated. It is found that the resulting CH3NH-G exhibits the best performance in interfering substances removal. Meanwhile, a multi-residue method is validated on 28 representative pesticide residues in four oil crops (rapeseed, peanut, sesame seeds and soybean). This method is based on modified QuEChERS sample preparation with CH3NH-G as reversed-dispersive solid phase extraction material and liquid chromatography-tandem mass spectrometry. Use of matrix-matched standards provides acceptable results for most pesticides with overall average recoveries between 70.5 and 100% and consistent RSDs<13%, except for pymetrozine, thidiazuron and diuron. In any case, this method still meets the 0.1-8.3 µg/kg detection limit needs for most pesticides and may be used for qualitative screening applications, in which any identified pesticides can be quantified and confirmed by a more intensive method that achieves >70% recovery.

Graphene-dispersive solid-phase extraction of phthalate acid esters from environmental water.

Graphene is a novel carbon nanomaterial with an ultra-high specific surface area. In this paper, we explored graphene as adsorbent for efficient enrichment of 15 phthalate acid esters (PAEs) under different water matrixes (ultrapure water, river and sea). A simple and inexpensive method of dispersive solid-phase extraction (DSPE) combined with gas chromatography-mass spectrometry (GC-MS) was used and acceptable results were provided for most PAEs with overall average recoveries between 71 and 117%. The extraction conditions such as the amount of graphene, the desorption solvent, adsorption time, desorption time and the solution pH were optimized. Finally, the method was applied for the determination of PAEs in environmental water samples including 9 rivers and 2 seas from 7 areas in China.

Determination and study on residue and dissipation of florasulam in wheat and soil under field conditions.

The residue and dissipation of florasulam in wheat and soil were determined by high performance liquid chromatography-tandem mass spectrometry. The dissipation half-lives for florasulam in soil were 0.66 days in Zhejiang and 0.64 days in Hebei. In wheat plant, half-lives of florasulam were 5.16 days in Zhejiang and 2.07 days in Hebei. The residues of florasulam in wheat grain, wheat straw and soil were below the detection limit (i.e., 0.01 mg/kg, the maximum residue level of florasulam). These results would be helpful in setting MRL guidance of florasulam in wheat in China.

A new bis(rhodamine)-based fluorescent chemosensor for Fe3+.

A new bis(rhodamine)-based fluorescent probe 4 was synthesized, and it exhibited high selectivity for Fe(3+) over other commonly coexistent metal ions in both 50% ethanol and Tris-HCl buffer. Upon the addition of Fe(3+), the spirocyclic ring of 4 was opened and a significant enhancement of visible color and fluorescence in the range of 500-600 nm was observed.