Ultra-performance Liquid Chromatography Tandem Quadrupole Research Articles

Ergot alkaloids: comparison of extraction efficiencies for their monitoring in several cereal-solvent combinations by UPLC-MS/MS.

To date, there are more than 80 ergot alkaloids identified; their distribution depends on different factors (e.g. geographic regions, host plants). These toxins can cause acute and chronic toxic effects on human health and commonly infect cereal crops such as triticale and rye, wheat, barley and oats. Considering the growing consumption of plant-based foods, the European Food Safety Authority has highlighted the need to develop risk assessment strategies. This work focused on the optimization of extraction efficiency, to quantify the main ergot alkaloids and their epimers, that are available on the market without any legal restriction (ergosine, ergocristine, ergocriptyne, ergocornine, ergosinine, ergocristinine, ergocriptinine and ergocorninine). Considering the quantification of 8 out of 12 regulated compounds by EU (sum of -ine and -inine forms), this approach can be defined as a screening method for a reliable estimation of the risk, specifically devoted to industrial stakeholders that can then possibly outsource to authorized external labs only the samples suspected of significant positivity. The effectiveness of three different extraction conditions (acidic, alkaline and neutral) followed by a rapid clean-up using dispersive solid-phase extraction with C18 sorbent was evaluated by ultra-performance liquid chromatography tandem quadrupole mass spectrometry (UPLC-MS/MS), resulting in a short chromatographic run (16min). The method was developed and validated in five different cereal production chains (rye, oat, wheat, wheat gluten and baby food). The applicability of the method was examined by analyzing a set of 54 samples, including also other cereals like spelt, tritordeum and triticale, and evaluating also some reference materials.

Banxia xiexin decoction prevents the development of gastric cancer.

In China banxia xiexin decoction (BXD) has been used in treating gastric cancer (GC) for thousands of years and BXD has a good role in reversing GC histopathology, but its chemical composition and action mechanism are still unknown. To investigate the mechanism of action of BXD against GC based on transcriptomics, network pharmacology, in vivo and in vitro experiments. The transplanted tumor model was prepared, and the nude mouse were pathologically examined after administration, and hematoxylin-eosin staining was performed. The active ingredients of BXD were quality controlled and identified using ultra-performance liquid chromatography tandem quadrupole electrostatic field orbitrap mass spectrometry (UPLC-Q-Orbitrap MS/MS), and traditional Chinese medicines systems pharmacology platform, drug bank and the Swiss target prediction platform to predict the relevant targets, the differentially expressed genes (DEGs) of GC were screened by RNA-seq sequencing, and the overlapping targets were analyzed to obtain the key targets and pathways. Cell Counting Kit-8, apoptosis assay, cell migration and Realtime fluorescence quantitative polymerase chain reaction were used for in vitro experiments. All dosing groups inhibited the growth of transplanted tumors in laboratory-bred strain nude, with the capecitabine group and the BXD medium-dose group being the best. A total of 29 compounds and 859 potential targets in BXD were identified by UPLC-Q-Orbitrap MS/MS and network pharmacology, RNA-seq sequencing found 4767 GC DEGs, which were combined with network pharmacology and analyzed 246 potential therapeutic targets were obtained and pathway results showed that BXD may against GC through the Phosphoinositide 3-kinase (PI3K)/protein kinase B (AKt) signaling pathway. In vitro cellular experiments confirmed that BXD-containing serum and LY294002 could inhibit the proliferation of GC cells, promote apoptosis, and inhibit the migration of GC cells by decreasing the expression of EGFR, PIK3CA, IL6, BCL2 and AKT1 in the PI3K-Akt pathway in MGC-803 expression. BXD has the effect of inhibiting tumor growth rate and delaying the development of GC. Its mechanism of action may be related to the regulation of PI3K-Akt signaling pathway.

Research Note: Pharmacokinetics of bromhexine hydrochloride in broilers after single oral and intravenous administration

The current study aimed to investigate the pharmacokinetics of bromhexine hydrochloride in broilers after single intravenous (IV) and oral (PO) administration at 2.5 mg/kg body weight (BW). The trial adopted a randomized, parallel-controlled design, where 20 twelve-wk-old broilers were randomly assigned to either the PO or IV group. Blood samples were collected at predetermined time points, and plasma was further separated for analysis. The bromhexine hydrochloride concentrations in plasma samples were determined using an ultra-performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS/MS) method. Noncompartmental analysis (NCA) using Phoenix software was conducted to analyze the concentration versus time data of bromhexine hydrochloride in every chicken. Subsequently, the main pharmacokinetic parameters between the 2 groups were statistically analyzed using SPSS software. Results from NCA revealed that after oral administration at 2.5 mg/kg BW, bromhexine hydrochloride exhibited slow absorption, reaching an average peak concentration of 32.72 ng/mL at 1.78 h. However, incomplete absorption was observed, with an absolute bioavailability of only 20.06% ± 10.84%. Additionally, bromhexine hydrochloride displayed wide distribution, with a steady-state distribution volume (VSS) of 22.55 ± 13.45 L/kg, and slow elimination, with a clearance (Cl) of 1.52 ± 0.38 L/h/kg. Furthermore, gender effects were assessed on the pharmacokinetics of bromhexine hydrochloride in broilers, revealing better absorption in male broilers compared to females. This disparity may be attributed to the faster blood flow and richer blood volume typically found in male broilers.

Qualitative Analysis Using UPLC-Q-TOF/MS and a Systematic Network Pharmacology-Based Strategy to Investigate the Active Constituents and Potential Mechanisms Against Breast Cancer in the Fruit Body of Sanghuangporus vaninii

Objective: To predict the pharmacodynamic material basis and mechanism of Chinese medicinal mushroom Sanghuangporus vaninii (Ljub.) L.W. Zhou & Y.C. Dai ( SV) against breast cancer based on ultraperformance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) and network pharmacology. Methods: We explored the compositional basis of SV using UPLC-Q-TOF/MS, then the potential targets and key pathways involved in the anti-breast cancer effect were predicted using a network pharmacology approach. Molecular docking was performed with the key compounds and the hub targets to confirm the results of the network pharmacology screening. Results: A total of 53 chemical components were identified, including 4 organic acids, 6 catechins, 13 pyranones, 13 flavonoids, and 17 fatty acids. 33 polyphenols and 144 corresponding targets were found to be significantly associated with its anti-breast cancer activity. Molecular docking results showed that the core compound could significantly bind to the core target. Conclusion: The anti-proliferative effect of SV against breast cancer could be attributed to a combination of multi-component, multi-target, and multi-channel mechanisms. The key active compound of SV in the treatment of breast cancer may be phellibaumin B, naringenin, hesperetin, sterubin, phelligrin A and phelligrin C, and the molecular mechanism may be related to the key targets MMP9, EGF, and EGFR, and that signaling pathways such as MAPK and PI3K-Akt may be responsible for SV-induced growth inhibition in breast cancer cells.

Chemical profiling and quality evaluation of Liuweizhiji Gegen-Sangshen oral liquid by UPLC-Q-TOF-MS and HPLC-diode array detector fingerprinting.

Liuweizhiji Gegen-Sangshen (LGS) oral liquid is a Chinese patent medicine that is widely used for the prevention and treatment of alcoholic liver disease in clinical practice. However, the chemical complexity of LGS has not yet been investigated. The aim of this study was to rapidly identify chemical constituents of LGS and establish a quality control method based on fingerprint and quantitative analysis. A comprehensive strategy was used by combining qualitative analysis by ultra-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and fingerprint analysis by high-performance liquid chromatography with diode array detection (HPLC-DAD). A total of 162 chemical components in LGS, including 91 flavonoids, 31 organic acids, and 20 phenolic compounds, were identified or preliminarily characterized in both positive and negative ion modes based on the UPLC-Q-TOF-MS results. Of these, 37 were confirmed with the reference standards. In fingerprint analysis, 23 peaks were chosen as common peaks and used to evaluate the similarity of different batches of LGS. Subsequently, a rapid quantification method was optimized and validated for the simultaneous determination of multiple chemical markers in LGS. The validated quantitative method was successfully used to analyze different batches of LGS samples. The proposed comprehensive strategy combining HPLC-DAD fingerprinting and multi-component quantification demonstrated satisfactory results with high efficiency, accuracy, and reliability. This can be used as a reference for the overall quality consistency evaluation of Chinese patent medicines.

Qualitative and quantitative analyses of chemical constituents in vitro and in vivo and systematic evaluation of the pharmacological effects of Tibetan medicine Zhixue Zhentong capsules.

Introduction: Zhixue Zhentong capsules (ZXZTCs) are a Tibetan medicine preparation solely composed of Lamiophlomis rotata (Benth.) Kudo. L. rotata is the only species of the genus Laniophlomis (family Lamiaceae) that has medicinal constituents derived from the grass or root and rhizome. L. rotata is one of the most extensively used folk medicines by Tibetan, Mongolian, Naxi, and other ethnic groups in China and has been listed as a first-class endangered Tibetan medicine. The biological effects of the plant include hemostasis, analgesia, and the removal of blood stasis and swelling. Purpose: This study aimed to profile the overall metabolites of ZXZTCs and those entering the blood. Moreover, the contents of six metabolites were measured and the hemostatic, analgesic, and anti-inflammatory effects of ZXZTCs were explored. Methods: Ultra-performance liquid chromatography-tandem quadrupole time-of-flight high-resolution mass spectrometry (UPLC-Q-TOF-MS) was employed for qualitative analysis of the metabolites of ZXZTCs and those entering the blood. Six metabolites of ZXZTCs were quantitatively determined via high-performance liquid chromatography The hemostatic, analgesic, and anti-inflammatory effects of ZXZTCs were evaluated in various animal models. Results: A total of 36 metabolites of ZXZTCs were identified, including 13 iridoid glycosides, 9 flavonoids, 9 phenylethanol glycosides, 4 phenylpropanoids, and 1 other metabolite. Overall, 11 metabolites of ZXZTCs entered the blood of normal rats. Quantitative analysis of the six main metabolites, shanzhiside methyl ester, chlorogenic acid, 8-O-acetyl shanzhiside methyl ester, forsythin B, luteoloside, and verbascoside, was extensively performed. ZXZTCs exerted hemostatic effects by reducing platelet aggregation and thrombosis and shortening bleeding time. Additionally, ZXZTCs clearly had an analgesic effect, as observed through the prolongation of the latency of writhing, reduction in writhing, and increase in the pain threshold of experimental rats. Furthermore, significant anti-inflammatory effects of ZXZTCs were observed, including a reduction in capillary permeability, the inhibition of foot swelling, and a reduction in the proliferation of granulation tissue. Conclusion: Speculative identification of the overall metabolites of ZXZTCs and those entering the blood can provide a foundation for determining its biologically active constituents. The established method is simple and reproducible and can help improve the quality control level of ZXZTCs as a medicinal product. Evaluating the hemostatic, analgesic, and anti-inflammatory activities of ZXZTCs can help reveal its mechanism.

UPLC-MS/MS Method for Simultaneous Determination of Valnemulin and Its Metabolites in Crucian Carp: In Vivo Metabolism and Tissue Distribution Analyses.

Valnemulin (VML) is a semi-synthetic pleuromutilin derivative widely used to treat animal bacterial diseases. However, no study has comprehensively evaluated VML metabolism in aquatic animals, including crucian carp. This study aimed to investigate VML metabolism in crucian carp. VML metabolites in crucian carp were quantified via intraperitoneal injection and analyzed via ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Three VML metabolites were detected in crucian carp via ultra-performance liquid chromatography-tandem quadrupole and time-of-flight mass spectrometry (UPLC-Q-TOF/MS) structural analysis. The enrichment and metabolism rules of the metabolites were summarized based on tissue distribution and concentration changes of the three metabolites. The metabolites were mainly found in the liver at 0.1 h after VML injection. The levels of the metabolites were abundant in the bile from 4 h to 12 h and in the skin after 72 h. The levels of the metabolites in the bile first increased, then decreased. The metabolism in the liver was completed at 72 h. The metabolites were detected in the skin following a 72 h period, which increased with time.

Integrated UPLC-Q-TOF-MS and network pharmacology approach-driven quality marker discovery of Danggui Shaoyao San for primary dysmenorrhea.

Danggui Shaoyao San (DSS), a famous prescription, has been clinically proved to be effective in treating primary dysmenorrhea (PD). Currently there is no valid quality control data available for DSS. The main aim of the current research was to explore quality markers (Q-markers) of DSS. The chemical constituents of DSS were qualitatively identified using ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) technology. On this basis, the targets of DSS and PD were predicted and screened using the TCMSP, SwissTargetPrediction, GeneCards, OMIM and TTD databases. Gene Ontology and Kyoto Encyclopedia of Genes and Genomes pathway analysis was performed on the core intersection targets using string and Cytoscape 3.7.1 software. Then molecular docking was conducted to screen the Q-markers of DSS in PD. A total of 126 chemical constituents, including 22 organic acids, 14 phthalides, 24 monoterpenoids, five sesquiterpene lactones, 22 triterpenoids, four phenylpropanoids and 35 other compounds were preliminarily characterized. According to network pharmacology prediction analysis, six compounds containing polyporenic acid C, senkyunolide P, alisol B 23-acetate, naringenin, gallic acid, ferulic acid and albiflorin were regarded as Q-markers of DSS. The present research established an integrative UPLC-Q-TOF-MS and network pharmacology method to discover the latent Q-markers of DSS and provided a theoretical data for the follow-up quality control of DSS.

Modulation of gut microbiota and lipid metabolism in rats fed high-fat diets by Ganoderma lucidum triterpenoids

Ganoderma lucidum triterpenoids (GP) have been reported to help prevent and improve hyperlipidemia. Modulation of the gut microbiota was proposed as underlying factor as well as a novel measure to prevent and treat hyperlipidemia. The effects of GP on high-fat diet (HFD)-induced hyperlipidemia and gut microbiota modulation were determined in rats. Ultra-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-QTOF MS-MS) indicated that GP were enriched with ganoderic acids G, B, H, A, and F. After feeding with GP supplementation, serum lipid levels including total triglyceride, total cholesterol, and low-density-lipoprotein cholesterol were significantly decreased in hyperlipidemic rats. Furthermore, administration of GP also has reversed the HFD-induced gut microbiota dysbiosis, including a significant increase in Alloprevotella and reduced proportion of Blautia. The result above suggests that GP would be developed as a functional food to ameliorate lipid metabolic disorders and hyperlipidemia.

Insights into the Kinetics, Theoretical Model and Mechanism of Free Radical Synergistic Degradation of Micropollutants in UV/Peroxydisulfate Process

The degradation of acyclovir (ACY) and atenolol (ATL) in the UV/peroxydisulfate (UV/PDS) process has been systematically considered, focusing on the degradation kinetics, theoretical models, and reaction pathways via applying a microfluidic UV reaction system. The removal efficiencies of ACY and ATL were >94.8%, and the apparent degradation rate constants (kobs) were 0.0931 and 0.1938 min−1 at pH 6.0 in the UV/PDS system. The sulfate radical (SO4•−) and hydroxyl radical (•OH) were identified as the major reactive radicals. The pH-dependent reaction rate constants of ACY and ATL with •OH and SO4•− were measured via the competing kinetics. Meanwhile, the contributions of •OH and SO4•− for ACY and ATL degradation were calculated by the radical steady-state hypothesis, and the results revealed that SO4•− occupied a decisive position (>84.5%) for the elimination of ACY and ATL. The contribution of •OH became more significant with the increasing pH, while SO4•− was still dominant. Moreover, ACY and ATL degradation performance were systematically evaluated via the experiments and Kintecus model under different operational parameters (Cl−, Br−, HCO3−, NOM, etc.) in the UV/PDS process. Furthermore, the plausible reaction pathways of ACY and ATL were elucidated based on the Fukui function theory and ultra-performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) analysis. The UV/PDS process has been demonstrated to be an efficient and potential application for micropollutants mitigation.

An integrated strategy for the comprehensive profiling of the chemical constituents of Aspongopus chinensis using UPLC-QTOF-MS combined with molecular networking

Context The extracts of Aspongopus chinensis Dallas (Pentatomidae), an insect used in traditional Chinese medicine, have a complex chemical composition and possess multiple pharmacological activities. Objective This study comprehensively characterizes the chemical constituents of A. chinensis by an integrated targeted and untargeted strategy using UPLC-QTOF-MS combined with molecular networking. Materials and methods The ultra-performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) combined with molecular networking-based dereplication was proposed to facilitate the identification of the chemical constituents of aqueous and ethanol extracts of A. chinensis. The overall strategy was designed to avoid the inefficiency and costliness of traditional techniques. The targeted compounds discovered in the A. chinensis extracts were identified by searching a self-built database, including fragment ions, precursor ion mass, and other structural information. The untargeted compounds were identified by analyzing the relationship between different categories, fragmentation pathways, mass spectrometry data, and the structure of the same cluster of nodes within the molecular network. The untargeted strategy was verified using commercial standard samples under the same mass spectrometry conditions. Results The proposed integrated targeted and untargeted strategy was successfully applied to the comprehensive profiling of the chemical constituents of aqueous and ethanol extracts of A. chinensis. A total of 124 compounds such as fatty acids, nucleosides, amino acids, and peptides, including 74 compounds that were reported for the first time, were identified in this study. Conclusions The integrated strategy using LC tandem HRMS combined with molecular networking could be popularised for the comprehensive profiling of chemical constituents of other traditional insect medicines.

Systematic investigation of the pharmacological mechanism for renal protection by the leaves of Eucommia ulmoides Oliver using UPLC-Q-TOF/MS combined with network pharmacology analysis

Bark is the traditional medicinal component of Eucommia ulmoides Oliver (E. ulmoides). However, the demand for E. ulmoides medicinal materials seriously limits their sustainability. To alleviate resource constraints, the bioactivity of E. ulmoides leaves and its pharmacodynamic basis were investigated. In the present study, extracts of E. ulmoides leaves were found to display potential renal protective properties in rat glomerular mesangial (HBZY-1) cells treated with high levels of glucose, suggesting that they possess potential factors capable of treating diabetic nephropathy. Ultra-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was used to comprehensively characterize the chemical components of E. ulmoides leaves. A total of 83 possible chemical components, including 12 iridoids, 13 flavonoids, 14 lignans, 20 phenylpropanoids, 14 phenolic acids, and 10 additional components, were identified in E. ulmoides leaves. Network pharmacology was used for a preliminary exploration of the potential mechanism of action of renal protection afforded by E. ulmoides leaves towards diabetic nephropathy. The network pharmacology results were verified using a series of biological experiments. The present study provided the basis for the comprehensive development and utilization of E. ulmoides leaves and the discovery of potential drugs.

Pharmacokinetics of 10-Hydroxy Mesaconitine in Rat Plasma by Ultra-Performance Liquid Chromatography-Tandem Quadrupole Mass Spectrometry.

Mesaconitine is the predominant active ingredient in Aconitum carmichaelii Debx. The compound 10-hydroxy mesaconitine is one known metabolite of mesaconitine and is toxic. In order to better understand its pharmacokinetics, UPLC-MS/MS was used in this paper to measure the concentration of 10-hydroxy mesaconitine in the plasma of rats after oral (5 mg/kg) and intravenous (0.1 mg/kg) administration of 10-hydroxy mesaconitine. The concentrations of 10-hydroxy mesaconitine in rat plasma measured in the standard curve covered the range of 0.3–60 ng/mL. The intraday and interday precisions of the samples of 10-hydroxy mesaconitine in rat plasma were lower than 15%. In addition, the accuracies ranged between 96.0% and 109.3%, the matrix effects ranged between 88.9% and 98.1%, and the recoveries were all higher than 79.1%. The AUC(0 − t) values were 23.6 ± 5.9 and 207.6 ± 72.9 ng/mL·h for intravenous and oral administration, respectively, and the bioavailability of 10-hydroxy mesaconitine was 17.6%. Lastly, t1/2 was 1.3 ± 0.6 h and 3.1 ± 0.4 h for intravenous and oral administration, respectively.

Degradation of norfloxacin by hydroxylamine enhanced fenton system: Kinetics, mechanism and degradation pathway

This study demonstrated a fast and efficient degradation of a typical antibiotic norfloxacin (NOR) in a hydroxylamine enhanced Fenton (HA-Fenton) system, which showed a higher catalytic activity over a wider pH range (3.0–9.0). The removal efficiency of NOR was 96% at following conditions: 10 mg/L NOR, 10 μM Fe2+, 1.0 mM H2O2, 0.4 mM HA and pH 5.0. The degradation rate of NOR in the HA-Fenton system (0.23 min−1) was 10.9 times of that (0.021 min−1) in Fenton system. The addition of HA to Fenton system accelerated the conversion of Fe3+ to Fe2+, leading to the high concentration of ·OH in the HA-Fenton system. Ten degradation transformation products were detected by ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometer (UPLC-QTOF-MS), consequently, three main degradation steps were proposed, including defluorination, quinolone group transformation, and defluorination and piperazinyl ring opening. Further analyses of NO3−, NO2− and F− after the reaction indicated that defluorination process was the crucial degradation step. The HA-Fenton system might offer an efficient alternative for degradation of antibiotics in wastewater.

Tongue Coating Bacteria as a Potential Stable Biomarker for Gastric Cancer Independent of Lifestyle.

Gastric cancer (GC) is one of the most common cancers, and the noninvasive diagnostic methods for monitoring GC are still lacking. Growing evidence shows that human microbiota has potential value for identifying digestive diseases. The present study aimed to explore the association of the tongue coating microbiota with the serum metabolic features and inflammatory cytokines in GC patients and seek a potential, noninvasive biomarker for diagnosing GC. The tongue coating microbiota was profiled by 16S rRNA and 18S rRNA genes sequencing technology in the original population with 181 GC patients and 112 healthy controls (HCs). Propensity score matching method was used to eliminate potential confounders including age, gender, and six lifestyle factors and a matching population with 66 GC patients and 66 HCs generated. Serum metabolomics profiling was performed by ultra-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) in the matching population. Random forest model was constructed for the diagnosis of GC. Linear discriminant analysis effect size (LEfSe) revealed that the differential bacterial taxa between GC patients and HCs in the matching population were similar to that in the original population, while the differential fungal taxa between GC patients and HCs dramatically changed before and after PSM. By random forest analysis, the combination of six bacterial genera (Peptostreptococcus, Peptococcus, Porphyromonas, Megamonas, Rothia, and Fusobacterium) was the optimal predictive model to distinguish GC patients from HCs effectively, with an area under the curve (AUC) value of 0.85. The model was verified with a high predictive potential (AUC = 0.76 to 0.96). In the matching population, eighteen specific HCs-enriched bacterial genera (Porphyromonas, Parvimonas, etc.) had negative correlations with lysophospholipids metabolites, and three of them had also negative correlations with serum IL-17α. The alteration of tongue coating microbiota had a possible linkage with the inflammations and metabolome, and the tongue coating bacteria could be a potential noninvasive biomarker for diagnosing GC, which might be independent of lifestyle.

Variation in Plant Morphology and Sinigrin Content in Ethiopian Mustard (Brassica carinata L.)

Ethiopian mustard (Brassica carinata) is mainly grown as a leafy vegetable and oilseed crop. Sinigrin is predominant glucosinolate in the leaves of Ethiopian mustard. It is hydrolyzed by enzyme myrosinase to produce bioactive product specifically allyl-isothiocyanates. Due to sinigrin content, Ethiopian mustard has a mild flavor and it is a healthy addition to human diet. However, sinigrin concentration depends on genotype. Understanding variations of plant morphology and sinigrin content may be the first step for crop improvement. According to the analyses of various plant characteristics among ninety nine Ethiopian mustard accessions, we found significant differences in plant height, chlorophyll content, and petiole length. In addition, sinigrin content was determined using ultra-performance liquid chromatography tandem quadrupole mass spectrometers/tunable ultraviolet detector (UPLC-TQS/TUV). We found a significant difference in sinigrin content among leaves of 94 Ethiopian mustard accessions. Except for petiole length, the sinigrin content was negatively correlated with leaf area, leaf width, number of primary branches, and plant height. This information will help Ethiopian mustard breeders in screening breeding lines for new accessions.

Rapid identification of constituents of Urtica hyperborea using UPLC-ESI-Q-TOF-MS/MS method

This paper deals with the application of ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry(UPLC-ESI-Q-TOF-MS/MS) method to rapidly determine and analyze the chemical constituents of methanol extract of Urtica hyperborea. We employed UPLC YMC-Triart C18(2. 1 mm×100 mm,1. 9 μm) column to UPLC analysis with acetonitrile-water(containing 0. 4% formic acid) in gradient as mobile phase. The flow rate was 0. 3 m L·min-1 gradient elution and column temperature was 30℃; the injection volume was 4 μL. ESI ion source was used to ensure the data collected in anegative ion mode. The chemical components of U. hyperborea were identified through retention time,exact relative molecular mass,cleavage fragments of MS/MS and reported data.The results indicated that a total of 31 compounds were identified,including 8 flavonoids,14 phenolic compounds,8 phenylpropanoids(4 coumarins and 4 lignans),and 1 steroidal compound,13 of which were confirmed by comparison. The UPLC-ESI-Q-TOF-MS/MS method could rapid identify the chemical components of U. hyperborea. The above compounds were discovered in U. hyperborea for the first time,which could provide theoretical foundation for further research on the basis of the pharmacodynamics of U. hyperborea.

Chemical composition and antioxidant capacity of extracts from the whole berry, pulp and seed of Hippophae¨ rhamnoides ssp. yunnanensis

In the present study, profiles of fatty acid, sn-2 fatty acid, triglyceride, phytochemical (including tocopherol/tocotrienol, phytosterol, flavonoid, carotenoid and polyphenol) and antioxidant capacity of extracts from the whole berry, pulp and seed of Hippophae¨ rhamnoides ssp. yunnanensis were investigated and compared. The distributions of fatty acid, sn-2 fatty acid and triglyceride that was identified using ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry (UPLC-Q-TOF/MS) showed obvious differences among the different parts of the ssp. yunnanensis. The whole berry and pulp extracts exhibited high flavonoid, carotenoid and polyphenol contents, whereas, the seed portion expressed high tocopherol/tocotrienol and phytosterol concentrations. Results deduced from this study demonstrated that ssp. yunnanensis is a rich source of unsaturated fatty acid and bioactive minor component, which should be further developed and utilized by breeders and planters.

Removal of ciprofloxacin from water by nitrogen doped TiO2 immobilized on glass spheres: Rapid screening of degradation products

Nitrogen doped TiO2 (N-TiO2) powders with different nitrogen doping dosages (urea) were prepared by sol gel method. Then, the powders were immobilized on the glass spheres by sodium silicate to improve its recyclability. The structure and morphological properties also were characterized. A common antibiotic ciprofloxacin (CIP) as water pollutant, was degraded to evaluate the photocatalytic activity of N-TiO2 immobilized on glass spheres. N-TiO2 sample with N/Ti weight ratio of 0.34% exhibits highest visible photocatalytic activity and the removal rate of CIP reached 90% in 90 min under visible light irradiation. The photocatalytic efficiency was hardly reduced after 5 cycle experiments, indicating that the recyclability of immobilized N-TiO2 was well. The kinetic model of degradation of CIP was confirmed as a first-order kinetic reaction model. The degradation products of CIP were analyzed by ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry (UPLC-Q-TOF MS). A database containing 49 kinds of the degradation products of CIP already reported in the papers was established to screen the UPLC-Q-TOF MS results. 17 kinds of degradation products were found and the possible degradation pathways to CIP were inferred. The toxicological properties of these degradation products were assessed by computer software simulation. In this study, a new, simple and stable immobilization method was used to prepare N-TiO2 immobilized on glass spheres, and a rapid screening method for the degradation products of CIP was established.

Design of Multifunctional Nanostructure for Ultrafast Extraction and Purification of Aflatoxins in Foodstuffs.

Aflatoxins (AFs) are a class of carcinogens, associated with liver cancers, that exist in foodstuffs. There are extremely low maximum limits of AFs in foodstuffs (0.025-20 μg·kg-1). Quick and sensitive detection of such low concentration of AFs in foodstuffs is dominated by the efficiency and selectivity of the AF enrichment process, which is extremely challenging although substantial efforts have been made in recent decades. Here we design and synthesize a multilayer nanoarchitecture composed of a broad-spectrum aflatoxin monoclonal antibody shell, chitosan middle layer, and magnetic bead core (denoted AF-mAb/CTS/Fe3O4). The efficiency of AF-mAb/CTS/Fe3O4 in extracting AFs has been found to be more than 60 times higher than both conventional immunoaffinity chromatography and solid-phase extraction. Furthermore, the nanocomposite displays excellent selectivity and good reusability as well as outstanding efficiency. When coupled to ultraperformance liquid chromatography-tandem quadrupole mass spectrometry, this new nanoarchitecture enables us to probe six AFs at concentrations as low as 0.003 μg·kg-1 in foodstuffs with free matrix effects, which is nearly 10 times smaller than the regulated maximum tolerated does. It is believed that the new nanoarchitecture will provide an efficient and fast pathway to detect AFs in foodstuffs to protect human being from some critical liver cancers.