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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]

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]

• Amino acids, nucleosides, nucleobases, sugars and protein in goji were analyzed. • Nutritional component profiles of goji from different regions were compared. • The regions located in Hetao plain produced goji with similar chemical profile. • Fructose and glucose are the main markers to distinguish goji from different areas. Goji berries are used as functional food for hundreds of years in Asia, Europe, North America and Austria, and are popular for nutritive properties in global. Commercial Goji berries are mainly produced in Ningxia, Xinjiang, Gansu, Qinghai and Inner Mongolia of China. However, the Goji berries produced in these regions exhibited different appearance and taste. Thus, characterization of the nutritional components in Goji berries produced in these regions could provide the guidance for application of them. In this study, 94 samples were collected, and a total of 20 amino acids, 17 nucleosides and nucleobases, 4 sugars and protein were determined by UHPLC-MS/MS, HPLC-ELSD or UV, and the variation was illustrated through heatmap clustering analysis, PCA and PLS-DA. The results showed that Goji berries from Xinjiang were rich in protein than the samples from other regions; those from Gansu and Ningxia were rich in amino acids, nucleosides and nucleobases; and those from Jiuquan of Gansu and Qinghai were rich in sugars. Heatmap clustering and PCA analysis results showed that all the samples exhibited a significant spatial aggregation, and the producing regions located along the Yellow River (belonging to the Hetao plain) produced Goji berries with the similar chemical profile. Additionally, PLS-DA analysis results showed that fructose and glucose were the predominant markers to distinguish Goji berries from different producing regions. [ABSTRACT FROM AUTHOR]

Graphical abstract Highlights • Pharmacokinetic study of quassinoid glycoside was performed for the first time. • Bruceoside A could serve as the precursor of the potent anticancer brusatol in vivo , rather than its direct deglycosylated metabolite bruceosin. • Quassinoid glycosides were proposed to be potential contributors to the anticancer properties of Fructus Bruceae. Abstract Bruceoside A, an abundant quassinoid glycoside in Fructus Bruceae, was chosen for the pharmacokinetic study. It is the first case report on the pharmacokinetic study of quassinoid glycosides so far. A sensitive, accurate, and repeatable UHPLC–MS/MS method was developed for the determination of bruceoside A and its major metabolite. The results showed bruceoside A could be transformed into the potent anticancer component brusatol in vivo , rather than its direct deglycosylated metabolite bruceosin. And the intestinal bacteria were proposed to take a potential role during such transformation. Based on the present study, it could be concluded that the quassinoid glycosides possessing weak activities in vitro could do contribution to the anticancer properties of Fructus Bruceae in vivo via transforming into more active metabolites. [ABSTRACT FROM AUTHOR]

Graphical abstract Highlights • Pharmacokinetic profiles of GAs and MPN after coadministration were obtained. • T max of MPN and its metabolites delayed and C max decreased. • Hhydroxylation metabolites of GA (15:1) and GA (17:1) were significantly reduced. • Glucuronidation metabolites of GA (15:1) and GA (17:1) were increased faster. Abstract Ginkgolic acids (GAs) and Ginkgotoxin (4′-O-methylpyridoxine, MPN) are main toxic compounds in Ginkgo biloba seeds which are widely used in the treatment of coughing in China. To evaluate the pharmacokinetics of GAs, MPN and their metabolites in rat plasma, a highly sensitive method followed by ultra-high-pressure liquid chromatography coupled with linear ion trap-Orbitrap tandem mass spectrometry (UHPLC-LTQ-Orbitrap-MS) has been developed and validated. The proposed method is selective, precise and accurate enough of MPN and its metabolites (4-pyridoxic Acid, pyridoxal, and pyridoxine) for the pharmacokinetic study. After oral administration of MPN, the plasma concentrations of MPN and its metabolites were increased rapidly. Meanwhile, an investigation was carried out to compare the interactions of the pharmacokinetic profiles of MPN and GAs. Five GAs and main metabolites of GA (15:1) and GA (17:1) were also analyzed by using our previous method. After coadministration GAs with MPN, T max of MPN delayed and C max decreased. Meanwhile, T max of 4-pyridoxic Acid, pyridoxal, and pyridoxine were also showed a certain degree of delay. The concentrations of hydroxylation products of GA (15:1) and GA (17:1) increased at a slower rate and the area under the curves was significantly reduced. However, glucuronidation metabolites of GA (15:1) and GA (17:1) were increased faster than administered of GAs alone. The interactions of the pharmacokinetic profiles of GAs and MPN in rat plasma after oral administration were obviously observed. [ABSTRACT FROM AUTHOR]

The root of Sophora flavescens Ait. has long been used as a crude drug in China and other Asian countries for thousands of years. The quinolizidine alkaloids and flavonoids are considered as the main bioactive components in this plant. To determine the distribution and content of the flavonoids in different organs of this plant, a rapid, sensitive and reproducible method was established using ultra-high-performance liquid chromatography coupled with a triple quadrupole electrospray tandem mass spectrometry. A total of sixteen flavonoids including five different types (isoflavones, pterocarpans, flavones, flavonols and prenylflavonoids) were simultaneously determined in 10 min. The established method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery and successfully applied in the methanolic extracts of S. flavescens parts (root, stem, leaf, pod and seed). The analysis results indicated that the distribution and contents of different type of flavonoids showed remarkable differences among the five organs of S. flavescens . This study might be useful for the rational utilization of S. flavescens resource. [ABSTRACT FROM AUTHOR]

• Fructo-oligosaccharides (FOS) were changed in Polygonatum cyrtonema rhizome process. • FOS increased following by a decrease over P. cyrtonema repeated steam-sun drying. • Four cycles of steam-heated air drying was found to be an optimal processing. • Heated air or infrared drying was not suitable to replace the traditional process. The rhizome of Polygonatum cyrtonema (Polygonati Rhizoma) is widely consumed as medicine-homology-food in Asia for its tonic effect, which can be enhanced by traditional steam-sun drying for nine cycles. However, the multi-constituents variation in this process was unclear, and the necessity of nine cycles should be further discussed. In this study, the multiple constituents, including saccharides, amino acids, nucleosides and bases, lipids, saponins, homoisoflavones and cinnamamides, in P. cyrtonema treated with sun drying, heated air drying, each cycle of steam-heated air drying, infrared drying and microwave drying were compared. The results showed that the content of total saccharides increased in samples from one to four cycles of steam-heated air drying (365.0–945.6 mg/g) and decreased from four to nine (945.6–288.0 mg/g). The content of fructose increased in samples from one to six cycles (29.9–234.7 mg/g) and decreased from six to nine (234.7–177.7 mg/g). The abundance of most phospholipids and free fatty acids increased continuously from one to nine cycles while most of the amino acids, nucleosides and bases showed continuous declining trend. Principal component analysis showed that the samples treated with one to four cycles were wider in distance than four to nine, indicating the chemical composition tending to be stable after fourth steaming. If taking total saccharides, fructose, and phospholipids as the major quality indicator, four cycles of steam-heated air drying processing should be the ideal postharvest processing method to obtain better taste, flavor and functionality. Samples treated with heated-air drying and infrared drying were far in distance from steaming ones by hierarchical cluster analysis, which means these processing methods were not suitable to replace the traditional steam-sun drying process. Collectively, the above results will not only provide novel processing methods that will obtain the high active ingredients for P. cyrtonema , but also shed light on the optimization of processing technology for the industrial production of medicinal crops which need nine cycles of steam-sun drying processing. [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]

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]

• UPLC-QTRAP®/MS2 was developed for simultaneous determination of 24 components. • The method was applied in determination of different regions and organs of LJ. • The differences of LJ between different regions and organs were remarkable. A rapid, sensitive and convenient analytical method of ultra-performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry (UPLC-QTRAP®/MS2) was proposed for the simultaneous determination of characteristic alkaline and acidic components covering many structure types including alkaloids, phenolic acids, phenylpropanoids and flavonoids in Leonurus japonicus Houtt. (LJ). The proposed method was first reported and validated by assessing the matrix effects, linearity, limit of detections, limit of quantifications, precision, repeatability, stability and recovery of target components. The developed UPLC-QTRAP®/MS2 was successfully applied to simultaneously determine all target compounds in 38 batches of LJ from 11 different producing regions in China and five organs (including root, caulis, branch, flower and leaf) of LJ from the same stand planting base in Jiangsu Province (China). The result showed that LJ in different regions with different geographical position would affect the accumulation of different compounds, and the significant discrepancies of some target compounds were also observed in different organs of LJ due to different biosynthetic pathway and enzymes in different organs. Furthermore, both hierarchical clustering analysis and principal components analysis were performed to classify the 38 batches of LJ samples from different producing regions on the basis of target compounds. As a result, the samples could be mainly clustered into different groups, which were similar with areas classification. Overall, the presented method would be helpful for the comprehensive utilization and development of LJ resources. [ABSTRACT FROM AUTHOR]