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Two new diterpenoids, dauricumins A (1) and B (2), together with two known aromatic meroterpenoids (3 and 4), were isolated from the petroleum ether soluble fraction of the stems from Rhododendron dauricum through an HPLC-MS-SPE-NMR combination strategy. The absolute configurations of 1 and 2 were elucidated by ECD calculations and [Rh2 (OCOCF3)4]-induced CD spectrum analysis. In a membrane potential FLIPR assay, confluentin (4) showed an agonistic effect on GABAA receptor (EC50 = 20 µM). [ABSTRACT FROM AUTHOR]

Highlights: [•] An HILIC–UHPLC-TQ-MS for determination of nucleosides, nucleobases and nucleotides. [•] Nucleotides could have good retentions and peak shapes with the proposed method. [•] The method is simple, rapid and sensitive than the previous methods. [•] The method was successfully applied to analysis of Ziziphus plants. [Copyright &y& Elsevier]

Abstract: The seeds of Sophora alopecuroides L. have been utilized as a crude drug in China for thousands of years. Quinolizidine alkaloids are the main bioactive components of this plant. To determine the distribution and content of quinolizidine alkaloids in different seed organs (seed coat and cotyledon), a reliable method has been established using ultra-high-performance liquid chromatography coupled with a triple quadrupole electrospray tandem mass spectrometry (UPLC–MS/MS). Seven constituents, namely cytisine, oxymatrine, oxysophocarpine, sophoridine, sophoramine, matrine, and sophocarpine, were simultaneously determined in 10min. The proposed method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery. The analysis results showed there were remarkable differences in the distribution and contents of the chemical markers between seed coat and cotyledon. The established approach could be helpful for the quality control of S. alopecuroides seeds, and also for the determination of this type class of alkaloids in other medicinal herbs. The present study can provide necessary information for the rational utilization of S. alopecuroides resources. [Copyright &y& Elsevier]

To discriminate the fruits of Ziziphus jujuba and Z. jujuba var. spinosa, a binary detector fingerprint was proposed and validated by utilizing HPLC coupled with two detection techniques of diode assay detection (DAD) and evaporative light scattering detection (ELSD). Using the data fusion method, the two sets of chromatographic data were combined to a fusion data set of fingerprints, which was further analyzed with chemometric methods of hierarchical clustering analysis (HCA) and principal component analysis (PCA). The results showed that the presented fingerprint obtained on DAD and ELSD could better represent the chemical characteristics of the jujube samples than that obtained at a single detector. With the aid of chemometric methods, this validated binary detector fingerprints method could be used as a powerful approach for discrimination of Z. jujuba and Z. jujuba var. spinosa. Furthermore, from the results of PCA, it was found that the main differences between the fruits of Z. jujuba and Z. jujuba var. spinosa were the content variances of the flavonoids and ursane-type triterpenic acids, so these compounds were promising to be selected as the markers for distinguishing these jujube fruits. [ABSTRACT FROM AUTHOR]

Abstract: The leaves of Ziziphus jujuba and Z. jujuba var. spinosa have been utilized as crude drugs for their health benefits in China for thousands of years. To control their quality, a reliable method based on high-performance liquid chromatography coupled with photo diode array and electrospray ionization tandem mass spectrometry detection (HPLC–PDA–ESI-MS/MS) was developed for exploration of the chemical profiles of these jujube leaves. As the results, fourteen constituents including three flavonoids, two saponins and nine triterpenic acids were identified or tentatively characterized. Then, twelve of them such as quercetin-3-O-rutinoside, zizyphus saponins I and II, ceanothic acid, alphitolic acid, maslinic acid, 2α-hydroxyursolic acid, zizyberanalic acid, epiceanothic acid, ceanothenic acid, betulinic acid, and oleanolic acid were selected as the chemical markers and were determined using an HPLC coupled with evaporative light scattering detection (ELSD) method. The separation was carried out on a Waters Sunfire C18 column with 0.2% acetic acid and acetonitrile as the mobile phase under gradient elution. The operating conditions of ELSD were set as 80°C for drift tube temperature and 2.7l/min for nitrogen flow rate. The developed method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery, and subsequently applied to evaluate the quality of eight batches of Z. jujuba and Z. jujuba var. spinosa leaves from different collections. [Copyright &y& Elsevier]

Abstract: A simple and sensitive HPLC–DAD method has been developed for the first time to simultaneously determine 10 triterpenoid acids (ceanothic acid, alphitolic acid, zizyberanal acid, zizyberanalic acid, epiceanothic acid, ceanothenic acid, betulinic acid, oleanolic acid, ursonic acid and zizyberenalic acid) in the dried fruit of Ziziphus jujuba (called Dazao) which has been widely used as one of the traditional Chinese medicines (TCMs). This HPLC assay was performed on a reversed-phase C18 column (250mm×4.6mm, 5μm) with the column temperature at 35°C. The mobile phase was composed of A (acetonitrile) and B (0.05% aqueous phosphoric acid, v/v). The flow rate was 1.0ml/min and the detection wave length was set at 205nm for reference compounds 1–9 and 238nm for reference compound 10. All calibration curves showed good linear regression (r 2 >0.9999) within the test range. The established method showed good precision and accuracy with overall intra-day and inter-day variations of 0.43–1.72% and 0.53–2.45%, respectively, and overall recoveries of 94.98–104.09% for the 10 compounds analyzed. The validated method was successfully applied for the simultaneous determination of the 10 triterpenoid acids in 42 batches of Dazao which contained 36 cultivars from 22 cultivation regions, and were investigated and authenticated as Z. jujuba. Hierarchical clustering analysis (HCA) and principal components analysis (PCA) were performed to differentiate and classify the samples based on the contents of the 10 triterpenoid acids. The presented HPLC–DAD method conjugated with chemometrics approach was demonstrated to be very helpful in using Dazao resources, and was possibly useful in chemotaxonomic characterization. [Copyright &y& Elsevier]

The enantiomers of eight pyrethroid insecticides have been separated by three polysaccharide-based chiral stationary phases (CSP), namely Chiralcel OD-R, Chiralpak AD, and Chiralcel OJ, both in reversed and normal phase modes. Deltamethrin, fenpropathrin, and lambdacyhalothrin could be baseline separated on Chiralcel OD-R in reversed phase mode with Rs values of 1.39, 1.29, and 1.17, respectively. However, the best separations for deltamethrin and fenpropathrin and tau-fluvalinate were achieved when the mobile phase was 15% of ethanol in water. Lambda-cyhalothrin enantiomers were separated using a mobile phase composed of 30% of acetonitrile : water (30 : 70 v/v). In normal phase mode, Chiralcel OJ gave better chiral separation for those pyrethroids than that of Chiralpak AD. The chiral separation conditions for eight pyrethroid insecticides have been discussed. [ABSTRACT FROM AUTHOR]

Molecular mechanics (MM) and molecular dynamics (MD) were used to study the π–π interaction between polynuclear aromatic hydrocarbon (PAH) and pyrene bonded silica phase. There was a good correlation coefficient (r = 0.9330, P = 2.4 × 10−4) between the logarithmic retention time (ln Tr) of PAHs and −ΔG. However, there was no linearity between the retention time of substituted benzene or naphthalene compounds on pyrene bonded silica stationary phase and ΔG. Quantitative structure–retention relationship (QSRR) had been used to study the relationship of retention time and microstructure. However, by using QSRR for the substituted benzene or naphthalene derivatives, we obtained good correlation coefficient between retention time and microstructures (r2 = 0.962, F-test = 104.198). The MM, MD, and QSAR are very useful methods to study the π–π interaction in chromatography. [ABSTRACT FROM AUTHOR]

Bufei Huoxue capsule (BHC) as a classic Chinese patent medicine formula, has the efficacy of tonifying the lungs and activating the blood. It has been extensively used in China for the treatment of chronic obstructive pulmonary disease (COPD) clinically. However, its mechanism is still unclear, which hampers the applications of BHC in treating COPD. The purpose of the present study was to demonstrate the protective efficacy and mechanism of BHC on COPD model rats by integrating serum metabolomics analysis and network pharmacology study. A COPD rat model was established by cigarette fumigation combined with lipopolysaccharide (LPS) airway drip for 90 consecutive days. After oral administration for 30 days, the rats were placed in the body tracing box of the EMKA Small Animal Noninvasive Lung Function Test System to determine lung function related indexes. Histopathological alteration was observed by H&E staining and Masson staining. The serum levels of inflammatory cytokine , matrix metalloprotein 9, and laminin were determined by ELISA kits. Oxidative stress levels were tested by biochemical methods. UHPLC-Q-TOF/MS analysis of serum metabolomics and network pharmacology were performed to reveal the bioactive metabolites, key components and pathways for BHC treating COPD. WB and ELISA kits were used to verify the effects of BHC on key pathway. BHC could improve lung function, immunity, lung histopathological changes and collagen deposition in COPD model rats. It also could significantly reduce inflammatory response in vivo, regulate oxidative stress level, reduce laminin content, and regulate protease-antiprotease balance. Metabolomics analysis found 46 biomarkers of COPD, of which BHC significantly improved the levels of 23 differential metabolites including arachidonic acid, leukotriene B4 and prostaglandin E2. Combined with the results of network pharmacology, the components of BHC, such as calycosin, oxypaeoniflora, (S)-bavachin and neobavaisoflavone could play therapeutic roles through the arachidonic acid pathway. In addition, the results of WB and ELISA indicated that BHC could suppress the expressions of COX2 and 5-LOX in lung tissues and inhibit the generation of AA and its metabolites in serum samples. Regulation of arachidonic acid metabolic pathway may be the crucial mechanism for BHC treating COPD. In summary, the studies indicated that BHC exhibited the protective effect on COPD model rats by anti-inflammatory and anti-oxidative properties through arachidonic acid metabolism pathway. This study provided beneficial support for the applications of BHC in treating COPD. [Display omitted] • BHC exhibits the protective effect on COPD model rats. • Anti-Inflammatory and anti-oxidant properties are exhibited by BHC. • BHC alleviates COPD by arachidonic acid metabolism pathway. [ABSTRACT FROM AUTHOR]

A chemical investigation of marine spongeJaspis stellifera, collected from the South China Sea, led to the isolation of four new isomalabaricane-type triterpenoids, jaspiferins C–F (1–4). The structures of those compounds were elucidated by extensive spectroscopic methods. Jaspiferin C (1), which has the six-membered carbon ring at the side chain, was discovered for the first time from the isomalabaricane-type triterpenoids. The hypothesis of a biogenetic pathway to generate jaspiferin C (1) was depicted. [ABSTRACT FROM PUBLISHER]

Amino acids are naturally occurring compounds in many edible or medicinal plants, which possess a variety of pharmacological effects on humans. The aim of this study is to develop and validate a hydrophilic interaction LC coupled with MS/ MS method for the absolute and relative quantification of amino acids without derivatization. The application of this method has been proven through 20 naturally occurring amino acids in 21 samples from different parts and phenological growth stage of Sophora alopecuroides. The method was performed on an ultra-high performance LC separation system coupled with ESI-MS on a triple quadrupole mass spectrometer. The proposed absolute quantitative method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery. The analysis results showed that S. alopecuroides is rich in free amino acids. In addition, relative quantitative determination of amino acids with several amino acids selected for the best accuracy was investigated. The accuracies of relative quantitative method for amino acids determinations suggest that it is feasible to quantify amino acids by the proposed relative quantitative determination method, which contributes to breaking through the choke point of lack of standards. [ABSTRACT FROM AUTHOR]

Five polysaccharide based chiral stationary phases have been used for separation of enantiomers of fourteen heterocyclic oxiranes. The polysaccharide based chiral stationary phases used in this study are Chiralak AD, Chiralpak AS, Chiralcel OD, Chiralcel OG, and Chiralcel OJ. From the chiral separation results, the chiral separation ability for the selected compounds show the order of Chiralpak AD > Chiralcel OD > Chiralcel OJ > Chiralcel OG > Chiralpak AS. Chiralcel OD appears to be quite versatile, since 8 out of 11 oxiranes with π-aromatic system were successfully resolved, yet no resolution was obtained for those oxirane derivatives, which lacks the π-aromatic system. Although Chiralcel OD is also versatile, it was not as effective; since the separation factors (α) are much smaller. The results indicate that dipole interactions have a strong impact on the retention mechanism, and extended π systems are essential. The spatial arrangement of the substituent groups around the analyte stereogenic center plays an important role in enantiomeric separations. The closer a group is to the chiral center, the more likely is the chiral recognition and enantioselectivity. [ABSTRACT FROM AUTHOR]

The herbal pair of Trichosanthis Pericarpium (TP) - Trichosanthis Radix (TR) can be seen in the famous formula "Beimu Gualou San". It is a commonly selected combination of medicinal herbs for the treatment of cough with lung heat. Both drugs are derived from Trichosanthes kirilowii Maxim, a medicinal plant known for its ability to clear heat, resolve phlegm, produce saliva, and alleviate dryness. However, the optimal combination ratio and active ingredients of TP-TR have yet to be determined. This study aims to investigate the optimal combination ratio of TP-TR and its anti-inflammatory active ingredients in cough treatment. A zebrafish (Danio rerio) inflammatory injury model and response surface method were applied in the present study to determine the appropriate proportion of TP-TR. Chemical constituents in TP-TR were identified using HPLC-ELSD and UPLC-MS/MS methods. Subsequently, a cough mouse model was created using an ammonia solution to evaluate the effectiveness of the optimal TP-TR ratio. Network pharmacology and intestinal flora sequencing were used to validate the anti-inflammatory components of TP-TR. The herbal pair of TP - TR at the ratio of 1:2 showed an optimal anti-inflammatory effect, with a composite inflammatory factor score of 119.645 in the zebrafish experiment. TP-TR combination facilitated the dissolution of glutamine, inosine, cytosine, isoquercetin, and other substances. In the animal model, the TP-TR (1:2) treatment significantly reduced the frequency of coughs and prolonged cough latency compared to the model group. Results of the network pharmacology indicated that inflammatory-related factors such as TLR4, STAT3, EGFR, and AKT1 played crucial roles in cough treatment with TP-TR, consistent with the validation experiment. The 16s rDNA sequencing results revealed a significant increase in the abundance of Clostridia_UCG-014, Lachnospiraceae , Christenella, Ruminococcus , and other species in the intestinal tract of mice after modelling. TP-TR (1:2) reduced the abundance of pro-inflammatory flora such as Clostridium_UCG-014 and Lachnospira , which were closely associated with L-lysine and trans-4-hydroxy-L-proline present in TP-TR according to correlation analysis. TP-TR may promote the dissolution of glutamine, thymidine, inosine, cytosine, isoquercetin, and other components through their combination, thereby regulating the abundance of Clostridium_UCG-014 and Lachnospira and exerting an antitussive effect. This study, for the first time, showed that TP-TR at a 1:2 ratio exhibits superior anti-inflammatory effects. In addition to inflammatory mediators like EGFR, TLR4, AKT1, and STAT3, gut microbes could also serve as potential regulatory targets of TP-TR in the treatment of cough. 2'-Deoxyguanosine monohydrate, L-lysine, L-leucine, γ-aminobutyric acid, L-valine, L-tryptophan, L-proline, trans-4-hydroxy-L-proline, L-methionine, uridine, 2'-deoxyinosine, guanosine, cucurbitacin B and cucurbitacin D were identified as its anti-inflammatory active ingredients. [Display omitted] • TP-TR at a 1:2 ratio exhibits superior anti-inflammatory effects. • TP-TR reduced the abundance of pro-inflammatory flora in cough-afflicted mice. • Amino acids were identified as anti-inflammatory active ingredients of TP-TR. [ABSTRACT FROM AUTHOR]

In the process of planting and harvesting of Rehmannia glutinosa, only the underground part is used, and a large number of stems and leaves that are considered non‐medicinal parts are usually discarded. Recent studies have shown that the chemical components in the leaves are similar to those identified in the roots. In this study, we selected leaves and roots from Rehmannia glutinosa at different growth stages and leaves from different cultivation regions to investigate the dynamic accumulation of three kinds of glycosides (catalpol, acteoside, and ajugol), six kinds of carbohydrates (rhamnose, fructose, sucrose, melibiose, stachyose, and verbascose), and acidic and neutral polysaccharides via rapid quantitative analysis technology, including ultra high performance liquid chromatography triple quadrupole tandem mass spectrometry, high‐performance liquid chromatography, and UV spectroscopy. The results showed that the Rehmannia glutinosa leaves also contained higher content of catalpol (3.81∼24.51 mg/g), ajugol (0.55∼10.23 mg/g), acteoside (1.34∼21.16 mg/g), monosaccharide/ oligosaccharides (7.71∼120.73 mg/g), and polysaccharides (5.63∼15.57%). In this study, we developed a new rapid and simple method for determination to clarify the distribution and dynamic accumulation of nine glycosides and saccharides in Rehmannia glutinosa leaves to provide a scientific basis for the discovery, development, and utilization of the resource value of Rehmannia glutinosa leaves. [ABSTRACT FROM AUTHOR]

A rapid and sensitive ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry method was established and employed to determine 21 nucleosides, nucleobases, and amino acids in 60 samples from different parts of Angelicae Sinensis Radix. The established methods were validated by good linearity (r2 > 0.9937), limits of detection (0.12–77.75 ng/mL), limits of quantitation (0.31–272.13 ng/mL), intra‐ and interday precisions (RSD ≤ 4.84%, RSD ≤ 6.26%), stability (RSD ≤ 5.92%), repeatability (RSD ≤ 7.14%), recovery (91.4–103.4%), and matrix effects (0.92–1.03). Chemical comparative analysis revealed that the content of total analytes in four parts of Angelicae Sinensis Radix were different, and exhibited the order: Head (14.89 mg/g) > Body (10.15 mg/g) > All (8.22 mg/g) > Tail (6.23 mg/g). Principal component analysis showed that the samples could be classified into four groups in accord with four different parts of Angelicae Sinensis Radix. The results could provide a scientific basis and reference for the quality control of Angelicae Sinensis Radix, and may be conducive to further research on the pharmacological activities of Angelicae Sinensis Radix. [ABSTRACT FROM AUTHOR]

Abstract: Salvia miltiorrhiza, a traditional Chinese medicine, is a widely used herbal medicine to treat cardiovascular and cerebrovascular diseases. In this study, ultraviolet (UV)–visible spectrophotometry and ultra‐high performance liquid chromatography with triple quadrupole tandem mass spectrometry analytical methods were used for rapid quantification of polysaccharides and 21 nucleosides and amino acids in S. miltiorrhiza to determine 17 samples of different tissues from different areas. Based on the total contents, hierarchical clustering analysis and principal components analysis were performed to classify these samples. The established methods were validated with good linearity, precision, repeatability, stability, and recovery. Chemical analysis revealed a higher content of total analytes in the sample of inflorescence from Nanjing (34.17 mg/g), sample of root and rhizome from Shaanxi (34.13 mg/g) and sample of stem and leaf from Nanjing (31.14 mg/g), respectively, indicating that root and rhizome from Shaanxi and the aerial parts from Nanjing exhibited the highest quality due to their highest content. In addition, contents of nucleosides and amino acids in the aerial parts (14.67 mg/g) were much higher than that in roots and rhizomes (9.17 mg/g). This study suggested that UV–visible spectrophotometry and ultra‐high performance liquid chromatography with triple quadrupole tandem mass spectrometry are effective techniques to analyze polysaccharides, nucleosides, and amino acids in plants, and they provided valuable information for the development and utilization value of the aerial parts of S. miltiorrhiza. This analysis would also provide useful information for the quality control of S. miltiorrhiza. [ABSTRACT FROM AUTHOR]

A highly sensitive method using ultra-high-pressure liquid chromatography coupled with linear ion trap-Orbitrap tandem mass spectrometry (UHPLC–LTQ–Orbitrap–MS) has been developed and validated for the simultaneous identification and quantification of ginkgolic acids and semi-quantification of their metabolites in rat plasma. For the five selected ginkgolic acids, the method was found to be with good linearities (r > 0.9991), good intra- and inter-day precisions (RSD < 15%), and good accuracies (RE, from −10.33% to 4.92%) as well. Extraction recoveries, matrix effects and stabilities for rat plasm samples were within the required limits. The validated method was successfully applied to investigate the pharmacokinetics of the five ginkgolic acids in rat plasma after oral administration of 3 dosage groups (900 mg/kg, 300 mg/kg and 100 mg/kg). Meanwhile, six metabolites of GA (15:1) and GA (17:1) were identified by comparison of MS data with reported values. The results of validation in terms of linear ranges, precisions and stabilities were established for semi-quantification of metabolites. The curves of relative changes of these metabolites during the metabolic process were constructed by plotting the peak area ratios of metabolites to salicylic acid (internal standard, IS), respectively. Double peaks were observed in all 3 dose groups. Different type of metabolites and different dosage of each metabolite both resulted in different T max . [ABSTRACT FROM AUTHOR]

A simple, sensitive and fast method for the simultaneous quantitation of 15 flavonoids in licorice based on an ultra high performance liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry had been established and validated in this study. The analysis was performed on an ACQUITY HSS T3 column with gradient elution using a mobile phase consisted of A (0.1% formic acid in water)/B (acetonitrile) at a flow rate of 0.4 mL/min. Satisfactory separation of these compounds was obtained in less than 9 min. All calibration curves showed good linearity ( r2 = 0.9940) during the test ranges. The precision, repeatability, accuracy, limit of detection and limit of quantification were also fully investigated. The validated method was successfully applied for the simultaneous quantitation of 15 flavonoids in 106 licorice samples which contained 83 batches of G. uralensis, 14 batches of G. glabra and 9 batches of G. inflata. Furthermore, multivariate statistical analysis (using principal components analysis) was performed to classify the samples based on the contents of the 15 analyzed compounds. The results showed that all of these licorice samples were rich in flavonoids, although their contents were obviously various, and the proposed method could serve as a prerequisite for quality control of licorice products. [ABSTRACT FROM AUTHOR]

Traditional Chinese Medicines (TCMs) derived from animal horns are one of the most important types of Chinese medicine. In the present study, a fast and sensitive analytical method was established for qualitative and quantitative determination of 14 nucleosides and nucleobases in animal horns using hydrophilic interaction ultra-high performance liquid chromatography coupled with triple-quadruple tandem mass spectrometry (HILIC-UPLC–QQQ-MS/MS) in selective reaction monitoring (SRM) mode. The method was optimized and validated, and showed good linearity, precision, repeatability, and accuracy. The method was successfully used to determine contents of the 14 nucleosides and nucleobases in 25 animal horn samples. Hierarchical clustering analysis (HCA) and principal component analysis (PCA) were performed and the 25 samples were thereby divided into two groups, which agreed with taxonomy. The method may enable quick and effective search of substitutes for precious horns. [ABSTRACT FROM PUBLISHER]

Three new polyunsaturated lipids, (6Z,9Z,12Z,15Z)-octadeca-6,9,12,15-tetraen-3-one (1), (6Z,9Z,12Z,15Z)-1-bromooctadeca-6,9,12,15-tetraen-3-one (2), and (Z)-ethyl docos-5-enoate (3), together with two known polyunsaturated lipids, 4(Z),7(Z),10(Z)-tridecatrienoic acid (4) and (6Z,9Z,12Z,15Z)-octadeca-1,6,9,12,15-pentaen-3-one (5), were isolated from the marine sponge Haliclona sp., which was collected from Guangxi, using HSCCC and HPLC methods. Chemical structures of the five compounds were elucidated by spectroscopic techniques. [ABSTRACT FROM AUTHOR]

The gorgonian Echinogorgia sassapo reticulata contains two new bioactive polyhydroxylated steroids, sassapols A (1), B (2), and five related known compounds (3–7). Compound 6 has been encountered for the first time in natural sources. The structures of these new compounds were defined by spectroscopic analysis. All the compounds (1–7) isolated from E. sassapo reticulata were tested for anti-inflammatory activity. Compounds 1, 3, 5, and 7 inhibited both the generation of leukotriene C4 and the degranulation reaction in mouse bone marrow-derived mast cells. [ABSTRACT FROM AUTHOR]

Highlights: [•] A HILIC-UPLC–TQ-MS method was developed for analysis of 17 nucleosides and nucleobases. [•] The profiles of nucleosides and nucleobases in EDC and CC were explored. [•] Protein precipitation with acetonitrile was performed on sample preparation. [•] Principal component analysis was performed to discriminate the samples. [Copyright &y& Elsevier]

Highlights: [•] Interaction analysis of multi-constituents in medicinal herbs during decocting in vitro. [•] Chemical fuzzy identification strategy was used for herbal constituent classification. [•] The approach is based on UPLC–TQ-MS, chemical fuzzy identification strategy and poly-proportion design. [•] The approach has been successfully applied to the interaction analysis of multi-constituents in kansui and licorice. [ABSTRACT FROM AUTHOR]

Abstract: Mactra veneriformis has been used as sea food and traditional Chinese medicine (TCM) for thousands of years in China. In the present study, a high performance liquid chromatograph coupled with photodiode array detector and electrospray ionisation-mass spectrometer (HPLC–DAD–ESI-MS) method was established for detection of the nucleosides and nucleobases in M. veneriformis from four aquaticultural area of Jiangsu during different harvest time of one year. The validated method was successfully applied to identifying 10 nucleosides and nucleobases in 48 M. veneriformis samples. Quantitative analysis showed that nucleosides and nucleobases are rich in all M. veneriformis samples. However, their contents vary in different areas and harvest times. Principal component analysis (PCA) was used to classify the 48 samples based on the contents of the nucleosides and nucleobases. As a result, the samples could be mainly clustered into four groups, which was similar as aquaticultural areas classification. Based on the results, present method might be applicable for the quality control of M. veneriformis, or even other marine shellfish aquiculture and their products, and the quality of M. veneriformis might be more related with aquaticultural areas. [Copyright &y& Elsevier]

A high performance liquid chromatographic method with diode array detection (DAD) was established for simultaneous determination of ten aromatic acids in five Siwu series decoctions (Xiongqiong decoction, Siwu decoction, Taohongsiwu decoction, Xiangfusiwu decoction, and Shaofuzhuyu decoction) and related 16 crude herbs. These ten compounds were analyzed simultaneously with a SunFire C18 column (4.6 mm × 250 mm, 5 µm) by gradient elution using 0.5% aqueous acetate acid (v/v)-methanol as the mobile phase; the flow rate was 1.0 mL/min. The sample was detected with DAD at 230, 254, and 323 nm and the column was maintained at 25°C. All the compounds showed good linearity (r2 > 0.9998) in the range of the test concentration. The precisions were evaluated by intra-day and inter-day tests, and relative standard deviation (RSD) values were reported within the range of 0.23–2.28% and 0.26–2.79%. The recovery studies for the quantified compounds were observed over the range of 94.8% and 104.6% with RSD values less than 3.29%. The validated method was successfully applied for the simultaneous determination of the aromatic acids contents in five formulae and 16 crude herbs, and some aromatic acids were identified for the first time in these crude herbs. The results also indicated that the contents of some aromatic acids varied greatly in different decocting process. This research provided some experimental data reference for clinical application of the relative herbs, and it could enhance the study of the compatibility rule of traditional Chinese medicine. [ABSTRACT FROM AUTHOR]

As traditional Chinese medicine (TCM) is gradually accepted by many countries, people pay much attention to the quality of herbal medicines. Because of the significant variation in active components in them, the quality control of herbal medicines is a very important issue. Nowadays, high-performance liquid chromatography (HPLC) fingerprint spectra (FPS) are widely used in identification and quality control of herbal medicines. This paper will analyze themethodology and their application in identifying and evaluating herbal medicines by means of HPLC FPS, which includes simple comparing, clustering, principal component analysis (PCA), and similarity analysis methods. [ABSTRACT FROM AUTHOR]

Abstract: A high performance liquid chromatography method coupled with diode array detection (HPLC-DAD) was developed for simultaneous determination of five major active flavonoids, two aristolactams and four main lignans in Saururus chinensis, namely rutin (1), isoquercitrin (2), quercetin-3-O-β-d-glucopyranosyl (1→4)-α-l-rhamnoside (3), quercitrin (4), quercetin (5), aristolactam A II (6), sauristolactam (7), dihydroguaiaretic acid (8), sauchinone (9), licarin A (10) and licarin B (11). The analysis was performed on an Agilent Eclipse XDB C18 column (4.6mm×150mm, 5μm) with gradient elution of 0.4% aqueous phosphoric acid and acetonitrile. The detection wavelengths were 280 and 360nm. All calibration curves showed good linearity (r 2 >0.9991) within test ranges. The method was reproducible with intra- and inter-day variation less than 3.2%. The recovery of the assay was in the range of 95.1–103.9%. The validated method was successfully applied for the analysis of the eleven bioactive compounds in seven samples from different harvesting seasons and significant variations were revealed. The results indicated that the developed method can be used as a suitable quality control method for S. chinensis and it should be harvested in August (fruiting period) for Jiangsu cultivation regions, taking the yield into consideration, with the highest amounts of lignans, relative higher amounts of flavonoids and lower amounts of aristolactams. [Copyright &y& Elsevier]