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Flavonoid glycosides exist widely in medicine herbs and often used as nutraceuticals because of their excellent bioactivity and low toxicity. For accurate quality control and bioactivity assessment of Sphaerophysa salsula, a rapid and productive method to isolate flavonoid glycosides is needed. Therefore, this work reports the development of a novel comprehensive strategy based on an online middle‐pressure chromatography and preparative high‐performance liquid chromatography for rapid enrichment and separation of flavonoid glycosides from S. salsula. First, the flavonoid glycosides were enriched using an online middle‐pressure chromatographic column containing stationary middle chromatogram isolated phase. During this process, the high‐volume injection of the extracting solution was realized by an empty precolumn positioned before the main chromatographic tower. Then, the compounds were separated through preparative high‐performance liquid chromatography with Megress C18. As a result, one new flavonol 3‐O‐glycoside (2) and two known flavonol 3‐O‐glycosides (1, 3) were targetedly isolated from S. salsula. The content of compounds 1–3 in S. salsula was 0.09, 0.11, and 0.18 wt%, respectively. Comparing to traditional enrichment and separation methods, our technique offers significantly shorter sample pretreatment time as well as high reproducibility. We believe that our separation method has a strong potential to be used for the processing of other medicinal plants. [ABSTRACT FROM AUTHOR]

We investigated the in vitro effects of Lactobacillus casei ZX633 on gut microorganism composition in infants with diarrhea. For this purpose, 103 feces samples from healthy infants (healthy group) and 300 diarrhea samples from infants (diarrhea group) were collected, and diarrhea feces were treated with L. casei ZX633, which was previously isolated from healthy infant feces (treatment group). We used microbial dilution plate methods, high performance liquid chromatography (HPLC) and high-throughput sequencing approaches to analyze viable main microorganism counts, short chain fatty acid (SCFA) concentrations, and intestinal microbiota composition in feces, respectively. Our data showed that L. casei ZX633 supplementation increased the numbers of Escherichia coli , yeasts, lactic acid bacteria (LAB) and aerobic-bacteria, raised propionic acid levels but reduced four other SCFAs, which are close to the healthy group. Alpha diversity results indicated that microbial diversity and richness decreased in treatment group. Bacterial community analyses revealed that microbial structures of the treatment group tended toward the healthy group; i.e., Escherichia-Shigella and Clostridioides abundance increased, and there was a reduction in the abundance of Streptococcus, Bacteroides, Enterococcus and Veillonella. In conclusion, L. casei ZX633 isolated from healthy infant feces, may be effective in improving infant diarrhea microbiota, potentially providing a new probiotic strain to reduce the incidence of diarrhea associated with bacterial disease in infants. [ABSTRACT FROM AUTHOR]

Abstract Lancea tibetica is an important traditional Tibetan medicinal plant that grows on the Qinghai-Tibet Plateau with great development potential in pharmaceutical industry. In this study, a combinative method using HPLC-DPPH and two-dimensional liquid chromatography has been developed to identify and separate antioxidants from Lancea tibetica. Under the target-guidance of HPLC-DPPH experiment, three antioxidant fractions from Lancea tibetica were recognized. Then, separation of the three fractions using two-dimensional semi-preparation liquid chromatography led to seven phenylpropanoids: (+)-pinoresinol-β-D-glucoside (1), isoacteoside (2), acteoside (3), tibeticoside (4),epipinoresinol (5), anthelminthicol (6) and phillygenol (7). As a result, seven major antioxidants in Lancea tibetica were isolated with more than 96% purity. Furthermore, in vitro bioassay against DPPH revealed compounds 1 – 7 with IC 50 values ranging from 6.16 ± 0.08 to 25.09 ± 0.11 (μM) and compounds 1 , 2 and 3 showed activities stronger than the two reference antioxidants (vitamin C, rutin), with IC 50 values of 6.16 ± 0.08, 8.93 ± 0.06 and 7.98 ± 0.05 (μM), respectively. Results of the present study indicated that the method was an efficient technique to systematically screen and isolate antioxidants from medicine crops. Graphical abstract Unlabelled Image Highlights • A novel screen and separation method for purification of antioxidants directly. • Seven antioxidants isolated from Lancea tibetica bioactivity-guided. • Isolated antioxidants with IC 50 values from 6.16 ± 0.08 to 25.09 ± 0.11 (μM). • The first report on antioxidant capacity of the compounds from Lancea tibetica. [ABSTRACT FROM AUTHOR]

Saussurea obvallata (DC.) Edgew. is a traditional Tibetan medicine used for the treatment of inflammation-related diseases, but the scientific validation was very limited. Aim of the study : This study aimed to rapid screen and targeted isolate cyclooxygenase-2 (COX-2) inhibitors from S. obvallata extract. An efficient ligand-fishing method based on affinity solid phase extraction (A-SPE) combining with HPLC was developed. The identified COX-2 inhibitors were separated using preparative liquid chromatography. In vitro COX-2 inhibition assays were employed to confirm the inhibitory activities of the isolated compounds. In addition, the effect of the isolated compounds on the production of prostaglandin E2 (PGE2) and the expression of COX-2 in LPS-induced RAW 264.7 were evaluated. A total of four phenylpropanoids, isolariciresinol, syringaresinol, pinoresinol and balanophonin were targeted isolated as COX-2 inhibitors with IC 50 values of 36.4 ± 2.6 μM, 23.1 ± 1.8 μM, 3.6 ± 0.3 μM and 12.1 ± 0.9 μM, respectively. The isolated compounds significantly inhibited LPS-induced NO production in a dose-dependent manner. And, the results of the inhibitory effect on the release of PGE 2 and the expression of COX-2 in LPS-induced macrophages were consistent with A-SPE analysis. The present work demonstrated that the developed A-SPE-HPLC method could successfully targeted isolated COX-2 inhibitors from S. obvallata extract. And, the isolation results indicated that the therapeutic effect of S. obvallata on inflammation-related diseases was partly based on the COX-2 active ingredients. [Display omitted] • A ligand-fishing method for targeted isolation of COX-2 inhibitors was developed. • Four phenylpropanoids were targeted isolated as COX-2 inhibitors. • The compounds have inhibitory effect on the release of PGE2 and COX-2 expression. • The effect in LPS-induced macrophages were consistent with A-SPE analysis. • The method could be used for isolation of COX-2 inhibitors from various products. [ABSTRACT FROM AUTHOR]

Pterocephalus hookeri, as a kind of popular traditional Tibetan medicine, is reputed to treat inflammatory related diseases. In the present work, a cyclooxygenase-2 functionalized affinity solid-phase extraction HPLC system was developed and combined with preparative-HPLC for rapidly screening and separating cyclooxygenase-2 ligand from P. hookeri extracts. Firstly, ligands of cyclooxygenase-2 were screened from extracts by affinity solid-phase extraction HPLC system. Then directed by the screening results, the recognized potential active compounds were targeted separated. As a result, the major cyclooxygenase-2 inhibitor of P. hookeri was obtained with a purity of >95%, which was identified as sylvestroside I. To test the accuracy of this method, the anti-inflammatory activity of sylvestroside I was inspected in lipopolysaccharide-induced RAW 264.7 cells. The results show that sylvestroside I significantly suppressed the release of prostaglandin E2 with dose-dependent, which was in good agreement with the screening result of the affinity solid-phase method. This method of integration of screening and targeted separation proved to be very efficient for the recognition and isolation of cyclooxygenase-2 inhibitors from natural products. [ABSTRACT FROM AUTHOR]

Abstract: The potential use of cigarette filters (CFs) as solid-phase extraction (SPE) adsorbents for the preconcentration of six fluoroquinolones (FQs) antibacterial agents prior to liquid chromatography was examined in this paper. In order to find a suitable procedure for extraction of the target FQs in one single step, various parameters probably affecting the extraction efficiency including the eluent kind and volume, sample flow rate, pH, ion strength and sample volume were systematically optimized. Under the optimized conditions, the target FQs could be easily extracted by the proposed SPE cartridge. Combination of SPE with HPLC/UV provided detection limits for different FQs of 2–5ngL−1 when 500mL of water sample was processed. The precision of the method, expressed as relative standard deviation, ranged from 4.1 to 6.3% for 2.5μgL−1 FQs. The recoveries of FQs spiked in environmental water samples ranged from 76 to 112%. The results obtained from the proposed method demonstrated that CFs-based solid-phase extraction combined with HPLC/UV was suitable for analyzing fluoroquinolones in water samples at ngL−1 concentration level. [Copyright &y& Elsevier]

Abstract: The potential of eggshell membrane (ESM) as a novel solid-phase extraction bio-adsorbent was investigated in the present study. The ESM with a unique structure of intricate lattice network showed a predominant ability to capture linear alkylbenzene sulfonates (LAS) as a model of organic pollutants by the hydrophobic interactions between ESM and LAS molecular at pH very close to the isoelectric point of ESM, which was similar to the most widely used trapping mechanism for SPE. Under the optimal conditions, the breakthrough capacities of the ESM packed cartridge for C10–C13 LAS homologues were found to be 30, 53, 50, and 43μgg−1, respectively. On the basis of high-performance liquid chromatography separation and UV detection of LAS homologues, the proposed system could respond down to 0.027ngmL−1 of LAS with a linear calibration range from 0.2 to 100ngmL−1, showing a good LAS enrichment ability of eggshell membrane biomaterial with high sensitivity, and could be successfully used for the detection of residual LAS in environmental water samples. The reproducibility among columns was satisfactory (RSD among columns is less than 10%). A comparison study with ESM, C8 and C18 as adsorbents for LAS demonstrated that ESM-based bio-adsorbent was advantageous over C8 and C18, the widely used traditional adsorbents. [ABSTRACT FROM AUTHOR]

• COX-2 immobilized silica was packed in affinity solid-phase extraction column. • Method of preparative HPLC guided by the ASPE-HPLC system was constructed. • Two COX-2 inhibitors were targeted isolated from P. hookeri with the method. • The method was valuable for obtaining COX-2 inhibitors in natural sources. Pterocephalus hookeri , a classical Tibetan herb, is mainly used to treat rheumatoid arthritis (RA) and contains various constituents potentially with cyclooxygenase-2 (COX-2) selective inhibition. A novel strategy for screening and target separating COX-2 inhibitors from the extracts of P. hookeri based on affinity solid-phase extraction (ASPE) column combined with preparative high-performance liquid chromatography (pre-HPLC) was successfully developed. The potential COX-2 inhibitors of P. hookeri were screened and recognized by the ASPE-HPLC system, which strategy is to analyze the compounds isolated by the ASPE column. Then, the active compounds were targeted separated by pre-HPLC according to real-time chromatograms. The control drugs celecoxib and glipizide were analyzed to verify the specificity and accuracy of the developed method. As a result, two pure compounds with COX-2 binding affinities were successfully separated from P. hookeri. They were characterized as swertisin and scopoletin using 1H- and 13C NMR spectroscopy, and the in vitro COX-2 inhibitory activities were verified. Compounds with COX-2 inhibitory activities could be screened and targeted separated from crude extracts by this strategy, which indicated that the proposed method was feasible, robust and effective for rapid separation of COX-2 inhibitors from natural products. [ABSTRACT FROM AUTHOR]

An offline preparative two-dimensional reversed-phase liquid chromatography/ hydrophilic interaction liquid chromatography coupled with hydrophilic interaction solid-phase extraction method was developed for the preparative isolation of flavonoid glycosides from a crude sample of Sphaerophysa salsula. First, the non-flavonoids were removed using an XAmide solid-phase extraction cartridge. Based on the separation results of three different chromatographic stationary phases, the first-dimensional preparation was performed on an XAqua C18 prep column, and 15 fractions were obtained from the 5.2 g target sample. Then, three representative fractions were selected for additional purification on an XAmide preparative column to further isolate the flavonoid glycosides. In all, eight flavonoid glycosides were isolated in purities over 97%. The results demonstrated that the two-dimensional liquid chromatography method used in this study was effective for the preparative separation of flavonoid glycosides from Sphaerophysa salsula. Additionally, this method showed great potential for the separation of flavonoid glycosides from other plant materials. [ABSTRACT FROM AUTHOR]

Abstract: In this paper, the potential use of multiwalled carbon nanotubes (MWCNTs) as solid phase extraction (SPE) adsorbent was evaluated for preconcentration of linear alkylbenzene sulfonates (LAS) using ion-pair (IP)-SPE with tetrabutylammonium hydroxide (TBAH). The LAS homologues present in the aqueous sample were ion-paired with TBAH and the solution was passed through the MWCNT cartridges. The analytes retained in the cartridge were eluted with methanol and the concentrated methanol extract was analysed by HPLC-UV. In order to obtain the satisfactory recovery of LAS homologues, various parameters including the type and amount of the ion-pair reagents, the desorption and enrichment conditions such as the effect of eluent and its volume, pH, the flow rate, the ultrasonic time of sample, and the volume of sample solution were systematically optimized. Under the optimal conditions, LAS homologues could be easily extracted by the proposed SPE cartridge. The favorable limits of detection (LOD) for LAS homologues were in the range from 0.02 to 0.03μgL−1, and the relative standard deviations (RSDs) were 1.55–2.54% for 10μgL−1 LAS (n =6). The proposed method has been successfully applied for the analysis of LAS homologues in aqueous environmental samples. A comparison study with ion-pair solid extraction on MWCNTs, C8 and C18 as adsorbents for LAS demonstrated that ion pair-based solid extraction on MWCNTs adsorbent was advantageous over C8 and C18, the widely used traditional adsorbents. [Copyright &y& Elsevier]

Abstract: Carbon nanotubes (CNTs) are a kind of new carbon-based nano-materials which have drawn great attention in many application fields. The potential of multi-walled carbon nanotubes (MWNTs) as solid-phase extraction (SPE) adsorbents for the preconcentration of environmental pollutants has been investigated in recent years. The goal of this work was to investigate the feasibility of MWNTs used as SPE adsorbents to enrich dichlorodiphenyltrichloroethane (DDT) and its metabolites including 1,1-dichloro-2,2-bis-(4′-chlorophenyl)ethane (DDD) and 1,1-dichloro-2,2-bis-(4′-chlorophenyl)ethane (DDE) at trace level which are typical persistent organic pollutants in environment. Parameters that maybe influence the extraction efficiency such as the eluent volume, sample flow rate, sample pH and the sample volume were optimized in detail. The experimental results showed the excellent linear relationship between peak area and the concentration of DDT and its metabolites over the range of 0.2–60μgL−1, and the precisions (RSD) were 2.3–2.5% under the optimal conditions. The detection limits of proposed method could reach 4–13ngL−1 based on the ratio of chromatographic signal to base line noise (S/N=3). Satisfied results were achieved when the proposed method was applied to determine the four target compounds in realworld water samples with spiked recoveries over the range of 89.7–115.5%. All these facts indicated that MWCNTs as SPE packing materials coupled to HPLC was an excellent alternative for the routine analysis of DDT and its metabolites at trace level in environment. [Copyright &y& Elsevier]