A simple liquid chromatography coupled with tandem mass spectrometry approach for the simultaneous quantification of thirteen compounds in rats following oral administration of raw and processed Fructus Xanthii: Application in a comparative pharmacokinetic study.

A simple and sensitive analysis using ultra high performance liquid chromatography with a tandem mass spectrometric system operated in selected reaction monitoring mode was developed for the determination of 11 phenolic acids, atractyloside, and carboxyatractyloside in rat plasma. The two classes of analytes were then separated on a Waters ACQUITY™ UPLC HSS T3 column (50 mm × 2.1 mm, 1.8 µm) using gradient elution with a mobile phase of 0.2% formic acid in water containing 10 mM ammonium acetate and methanol. Detection was accomplished by selected reaction monitoring scanning via an electrospray source operating in negative ionization mode. The calibration curve was linear (R2  = 0.990) over a concentration range of 1.20-3500 ng/mL, while the validated lower limit of quantification was 1.20 ng/mL. The precision varied from 0.84 to 4.62%, and the accuracy varied within ±5%. The method proved robust with sample freezing and thawing and with short- and long-term sample storage. The established method was used for simultaneous quantification and was successfully used for the first time for the pharmacokinetic evaluation of 13 compounds after the intragastric administration of raw and processed Fructus Xanthii in rats. The results indicated that processing affects the absorption and metabolism of Fructus Xanthii extract. Importantly, the results also indicated the importance of processing for the clinical application of traditional Chinese medicine.

Fructus Xanthii and Magnolia liliiflora Volatile Oils Liposomes-Loaded Thermosensitive in situ Gel for Allergic Rhinitis Management.

Purpose: The aim of the present study was to fabricate a Fructus Xanthii and Magnolia liliiflora volatile oils liposomes-loaded thermosensitive in situ gel (gel/LIP/volatile oil) for effectively treating allergic rhinitis via intranasal administration. Patients and Methods: Particle size, polymer dispersity index (PDI), entrapment effectiveness, and cumulative drug permeation of the developed liposomes were assessed. Then, a thermoreversible in situ gel was created using the liposomes loaded with volatile oils of Fructus Xanthii and Magnolia liliiflora. The effectiveness of this treatment for allergic rhinitis was confirmed by evaluating nasal symptoms, and hematological results, after injecting the formulation into the ovalbumin (OVA)-sensitized mice, we conducted hematoxylin-eosin staining (HE) and immunohistochemistry to evaluate the outcomes. The effects of the gel/LIP/volatile oil formulation for nasal delivery of volatile oil in the treatment of rhinitis were then assessed. Results: The average particle size was 95.1 ± 3.6 nm, and the encapsulation efficiencies of Fructus Xanthii and Magnolia liliiflora volatile oils were 70.42 ± 5.41% and 67.10 ± 6.08%, respectively. Drug loadings of Fructus Xanthii and Magnolia liliiflora volatile oils were 9.10 ± 0.98% and 16.10 ± 1.03%, respectively. The binary formulation produced a gel rapidly in the nasal cavity with a strong mucosal adherence at a temperature of delivering volatile oil to the nasal mucosa steadily and continuously. After nasal administration, the gel/LIP/volatile oil sustained the volatile oil delivery into the mucosa. In comparison to the monolithic formulations, the gel/LIP/volatile oil binary formulation exhibited superior performance in terms of drug delivery capability and pharmacodynamic effects. Conclusion: This binary preparation displayed the ability to deliver drugs to the nasal mucosa and exhibited positive pharmacodynamic effects in treating OVA-induced rhinitis in mice. As a result, it has the potential to serve as a delivery platform for Traditional Chinese medicine in the treatment of allergic rhinitis.

Fructus Xanthii-Inspired Low Dynamic Noise Dry Bioelectrodes for Surface Monitoring of ECG.

The microstructured surfaces of bioelectrical dry electrodes are important aspects of dry electrode design. However, traditional surfaces for microstructured bioelectrical dry electrodes are costly to produce and require complex fabrication methods. In this study, a novel stacked-template method is proposed for the first time, rapidly producing microstructured dry electrodes at a low cost and with a large surface area. Three types of microstructured Ag/AgCl thermoplastic polyurethane (TPU) electrodes with a Fructus xanthii-inspired barb structure (FXbs) are prepared using this method; then, the dynamic friction, hair interference resistance, electrochemical, and electrocardiogram (ECG) signal acquisition performance of the electrodes are tested, and the dynamic noise characteristics of the electrodes are comprehensively evaluated with simulated instruments. Compared to the plate structure, the dynamic friction coefficient of the FXbs electrode improved by about 38.8%, exhibiting strong hair interference resistance. In addition, the FXbs electrode exhibits low dynamic noise and comparable performance to the wet electrode, in terms of signal acquisition, when it is tested using simulated instruments. Therefore, the prepared FXbs electrode increases the friction coefficient between the electrode and the skin, which effectively resolves issues related to dynamic noise in bioelectrical signals, making it suitable for dynamic measurements.

Chemometrics coupled with UPLC-MS/MS for simultaneous analysis of markers in the raw and processed Fructus Xanthii, and application to optimization of processing method by BBD design.

BACKGROUND: As a widely used toxic traditional herbal medicine, the quality of the Fructus Xanthii must be well controlled to ensure the clinical therapeutic efficacy and safety. AIMS: A rapid, and sensitive using ultra-high performance liquid chromatography to triple quadrupole tandem mass spectrometry (UPLC-MS/MS) in selected reaction monitoring (SRM) mode was developed and validated for simultaneous quantitation of determination active and toxic ingredients form processed by stir-frying and raw materials of Fructus Xanthii. METHODS: Chromatographic separation of all targeted compound was performed on Waters ACQUITY UPLC HSS T3 column (50 mm × 2.1 mm, 1.8 µm). Moreover, the method was successfully applied in thirty-six samples of Fructus Xanthii collected from different sources in China. The processing method was optimized through Box-Behnken statistical design and response surface methodology. RESULTS: In this work, chemometrics was able to successfully discriminate and classify among samples. The optimal incubation conditions were as follows: under heating in a pot at 295 °C, medicine at 120 °C for 11.0 min with flipping frequently. CONCLUSIONS: Therefore, the established UPLC-QQQ-MS method in combination with chemometric analysis provides a rapid, flexible and reliable method for quality assessment of Fructus Xanthii. Importantly, the optimized experimental value of the processing process provides the basis for future research.

Anti-allergic rhinitis effects of caffeoylquinic acids from the fruits of Xanthium strumarium in rodent animals via alleviating allergic and inflammatory reactions

Abstract The fruits of Xanthium strumarium L., Asteraceae, have been used for various diseases in Chinese folk medicine, including allergic rhinitis, tympanitis, arthritis, ozena etc. The current study was aimed to investigate the therapeutic effects of caffeoylquinic acids from fruits of X. strumarium on allergic rhinitis in animals. The toxicity test indicated that the caffeoylquinic acids have no obvious toxicity. By using HPLC assays combined with reference standards, ten caffeoylquinic acids were identified as the predominant constituents. Anti-allergic activities of the caffeoylquinic acids were evaluated using passive cutaneous anaphylaxis test and Schultz-Dale test; dimethylbenzene induced ear edema test was performed to evaluate its anti-inflammatory effect. Then, the allergic rhinitis model in rats was established to evaluate the therapeutic effects of the caffeoylquinic acids against allergic rhinitis with the following indexes: allergic rhinitis symptom scores, serum levels of pro-inflammatory cytokines, histopathological examination, and histamine release. Our study revealed that the caffeoylquinic acids showed obvious anti-allergic and anti-inflammatory properties, and its treatments were beneficial for ameliorating the nasal symptoms, decreasing pro-inflammatory cytokines, and inhibiting the releases of histamine. Collectively, the caffeoylquinic acids might be utilized as effective and safe disease therapeutic agents for allergic rhinitis.

Anti-allergic rhinitis effect of caffeoylxanthiazonoside isolated from fruits of Xanthium strumarium L. in rodent animals.

The fruits of Xanthium strumarium L. (Asteraceae) have been used extensively in China for treatment of various diseases such as allergic rhinitis (AR), tympanitis, urticaria and arthritis or ozena. This study was designed to systemically investigate the effects of the caffeoylxanthiazonoside (CXT) isolated from fruits of X. strumarium on AR in rodent animals. Animals were orally administered with CXT. Anti-allergic activity of CXT was evaluated by passive cutaneous anaphylaxis test (PCA); acetic acid-induced writhing tests were used to evaluate the analgesic effects of CXT; acetic acid-induced vascular permeability tests were performed to evaluate anti-inflammatory effect of CXT. Then, the model AR in rats was established to evaluate the effects of CXT on AR with the following tests: the sneezing and nasal scratching frequencies, IgE level in serum, and histopathological examinations. Our results demonstrated that CXT had favorable anti-allergic, anti-inflammatory and analgesic effects. Additionally, we found that CXT was helpful to ameliorate the nasal symptoms and to down-regulate IgE levels in AR rats. Thus, we suggested that CXT can be treated as a candidate for treating AR.

Simultaneous determination of 5 phenolic acids in fried Fructus xanthii from different production sites and its dispensing granules by using ultra-pressure liquid chromatography.

BACKGROUND: To establish a ultra-pressure liquid chromatography (UPLC) method for the determination of 5 phenolic acids including neochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, and cynarin in fried Fructus xanthii from different production sites and its dispensing granule. MATERIALS AND METHODS: An Acquity BEH C18 chromatographic column (100 mm × 2.1 mm,1.7 µm) was used to perform the determination, which was maintained at 40°C throughout the analysis. Mobile phase was composed of methanol and water containing 0.1% phosphoric acid (v/v) with flow rate at 0.4 mL/min under gradient elution, and detection wavelength was set to 325 nm for monitoring the separation. RESULTS: Neochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, and cynarin have shown good linearity (r (2)≥0.9997) within 0.959-239.75, 0.9408-235.2, 0.1638-40.95, 0.6744-67.44, and 0.47-117.5 µg/mL, and their average recoveries were 100.09%, 99.98%, 101.74%, 99.83%, and 99.63%, respectively. CONCLUSION: The UPLC method established in this study was rapid, and of good accuracy, repeatability and resolution, and hence can assist in the control quality of fried Fructus xanthii as well as its dispensing granule in an efficient manner.

Numerical taxonomy of origin plants of Fructus Xanthii and identification of its crude drug / 第二军医大学学报

Objective: To conduct a numerical taxonomy research on the origin plants of Fructus Xanthii and to identify this crude drug, so as to provide evidence for the classification, identification and germplasm optimization of Xanthium genus. Methods: Fruits of Xanthium plants from 25 populations in China were collected and cultivated in the same location. Their growing conditions and morphological characteristics were observed after seedling emergence. And 20 taxonomic characters of the plants such as growth cycle, height of the whole plant, length of leafstalk, length and density of involucre, thorn, length of beak and color of ripe fruits, etc. were selected for detailed observation, recording and analysis. Original data matrix X= {Xii} 25×20 was established by means of 25 operational taxonomic units(OTU) and related 20 groups of characteristic data. The established matrix was analyzed using hierarchical cluster analysis on SPSS 13.0 software. Results and Conclusion: The origin plants of Fructus Xanthii from 25 populations of China fell into four groups, largely consistent with the morphological identification results of this study. The first group was identified as Xanthium sibiricum, the second as X. mongolicum, the: third as X. sibiricum var. subinerme, and the fourth was temporarily named as Shenzhen-type cocklebur Xanthium sp.. The Shenzhen-type cocklebur was special in some taxonomic characters and was possibly a cultivated variety of Xanthium genus. The origin plants of Fructus Xanthii in China can be systematized into 3 species and 1 type, which has been added to the existing taxonomic criteria. The cluster analysis method in this study can be applied for discrimination of Xanthium plants and crude drugs.

Application of Accelerated Solvent Extraction(ASE) for the Extraction of Compounds in Fructus Xanthii / 中药新药与临床药理

Objective To establish a method for extracting compounds in Fructus Xanthii by accelerated solvent extraction(ASE),and to simultaneously determine the compounds by GC-MS.Methods The extraction was performed by ASE in which the conditions were optimized by orthogonal test,then the compounds in different extracts with different polarity were determined by GC-MS.Results The optimized conditions of ASE for compounds in Xanthium sibiricum fruits were as follows: petroleum ether,ethyl acetate and methanol as extracting solvent in turn in 33 mL extracting tube and the volume of solvent being 65 mL;6 g sample,9 MPa of extracting pressure,90 ℃of extracting temperature,5 min of extracting time,two cycles and one time for each extraction.The GC-MS conditions were as follows: 1 ?L extract was analysed by GC-MS(Shimadzu Model QP-2010) instrument fitted with a flame ionisation detector,separation was achieved on a DB-5ms,DB-17ms and DB-WAX column(J&W Scientific,30 m,0.25 ?m id film thickness,1.4 ?m,USA) respectively,the column temperature was maintained at 60 ℃for 3 min and increased to 250 ℃,the scanning range was from m/z 40 to m/z 700(scanning interval: 0.5 s),and the compounds were identified by searching NIST and Wiley registry of mass spectral data.Conclusion There are 61 compounds found in the petroleum ether extract and in which 48 are identified,22 in the ethyl acetate extract and 18 identified,as well as 34 in the methanol extract and 29 identified with the methods of optimized ASE combined with GC-MS.