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In this study, a rapid and highly sensitive ultra high performance liquid chromatography with triple quadrupole mass spectrometry method with the mobile phase of acetonitrile and 0.1% aqueous formic acid was established and successfully applied to comparatively analyze main active components after their compatibility. Besides, the effects of Scutellariae Radix, Coptidis Rhizoma and combined extracts on type 2 diabetic rats induced by high‐fat diet along with low dose of streptozocin were investigated. Under the optimized chromatographic conditions, good separation of seven target components was achieved within 12 min. All calibration curves exhibited good linearity (R2 ≥ 0.999). The relative standard deviation of precision, repeatability and stability varied from 0.69 to 2.23, 0.98 to 2.56, and 0.92 to 2.57%, respectively. The recovery ranged from 91.11 to 105.35%. The contents of seven active components were notably reduced after compatibility; however, the hypoglycemic effect of combined extracts was stronger than single drug by decreasing the activities of fructose‐1,6‐bisphosphatase, glucose 6‐phosphatase, phosphoenolpyruvate carboxykinase and increasing the activities of glucokinase, phosphofructokinase, pyruvate kinase. Accordingly, the established analytical method was accurate and sensitive enough for quantitative evaluation of seven investigated compounds. Moreover, the combined extract had definite effects on type 2 diabetes through multiple components against multiple targets. [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]

An ultra high performance liquid chromatography coupled with a triple quadrupole mass detection and electrospray ionization mass spectrometry method has been established for the simultaneous determination of the 14 nucleosides and nucleobases, 24 amino acids and two main alkaloids in mulberry leaf. In this method, a complicated mobile phase, the flow rate of which was 0.4 mL/min, was applied to the gradient elution, which provided a satisfied separation of the 40 compounds. The present method was validated, and sufficient reproducibility and accuracy were obtained for the quantitative measurement of the 40 compounds. The method was subsequently applied to ten mulberry leaves and the results showed that almost all of these samples were rich in nucleosides, nucleobases, amino acids, and alkaloids. The proposed method, which is convenient and economical, could serve as a prerequisite for the quality control of mulberry leaf herbs and be applied analogously to other Chinese medicines. [ABSTRACT FROM AUTHOR]

Highlights • A hierarchical extraction method was established for determination flavonoids and triterpenes in T. kirilowii. • An UHPLC-MS/MS method was established for quantification multiple compounds. • Reveal the distribution of resource components in different parts of T. kirilowii. • The results could be useful for the rational utilization of T. kirilowii. Abstract Trichosanthin (root of Trichosanthes kirilowii Maxim.) has received much attention, but T. kirilowii has received little systematic analysis. A comprehensive evaluation of flavones and triterpenes in nine different parts of T. kirilowii would, thus, be of value to fully understand the potential medicinal properties of T. kirilowii. A hierarchical extraction—simultaneous determination method was established, which based on different types of components had different response on the MS detector. The hierarchical extraction method extracted 3, 29-dibenzoyl rarounitriol solely, which response lowly on the MS detector in the mixture of one step extract, in order to obtain accurate results in the next UHPLC-MS/MS assay. By this method, ten flavones, three tetracyclic triterpenoids, and one pentacyclic triterpenoid in the extracts of T. kirilowii were determined. The results showed the level of flavonoids in leaves was higher than those in the other samples, tetracyclic triterpenoids mainly existed in root and root bark, and pentacyclic triterpenoid, especially 3, 29-dibenzoyl rarounitriol was concentrated in the seed kernel. According to principal component analysis, the F values of the leaves of all varieties were generally greater than those in other parts. The leaves might provide a supplementary source of flavonoids, and the root and root bark could be a good choice for tetracyclic triterpenoids. The analysis results revealed the distribution of flavones and triterpenes in different parts of T. kirilowii and provided reference for the research and rational utilization of T. kirilowii. [ABSTRACT FROM AUTHOR]

Highlights • A UPLC-MS/MS method was established for determination volatile in herb pair. • Response surface analysis was employed to explain the herb–herb interactions. • The results were positive to Cyperi Rhizoma herb pair based products development. Abstract Cyperi Rhizoma (Xiangfu) combined with either Angelicae Sinensis Radix (Danggui) or Chuanxiong Rhizoma (Chuanxiong) are herb pairs that are commonly used in clinical settings. To illustrate the herb–herb interactions that occur when extracts from these herbs are obtained together, ultra-high-performance liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry and response surface analysis were used. Volatile components, α-cyperone, nootkatone, ligustilide, senkyunolide A and senkyunolide I, were accurately identified with high precision. When Xiangfu was combined with Danggui at a 1:1 ratio, or with Chuanxiong at a 1:1 or 2:1 ratio, the dissolution rates of α-cyperone and nootkatone from the herbs were greatly increased, compared to those obtained from Xiangfu extract alone. The dissolution rates of ligustilide, senkyunolide A and senkyunolide I from Danggui or Chuanxiong changed proportionally to changes in the ratios of Xiangfu with either Danggui or Chuanxiong. Response surface analysis results presented polynomial regression equations between the dissolution of tested compounds and the corresponding input variables, including compatibility proportions and solvent dosage. Based on the predicted results from response surface analysis, a combination of Xiangfu with Chuanxiong at a ratio of near 1:1, or with Danggui at 1:2, resulted in the maximum dissolution of five volatile components. Our established method could be applied to herb–herb interaction research, and the results may provide a scientific basis for the development of Cyperi Rhizoma–Chuanxiong Rhizoma, or Cyperi Rhizoma–Angelicae Sinensis Radix-based formulas and products. [ABSTRACT FROM AUTHOR]

A novel and generally applicable approach was established to hierarchically identify the bioactive components of a medicinal herb by preparative high-performance liquid chromatography (prep-HPLC) and a selective knock-out strategy. In this study, the targeted components of an herbal medicine were separated and knocked out using prep-HPLC. Subsequently, the contributions of the different target components to the overall effect of the medicinal herb were comparatively evaluated and differentiated by a heat map and a 3D score plot. This approach was successfully applied to investigate the bioactive constituents of safflower. The contributions of 11 components to the overall effect of safflower were as follows: anhydrosafflor yellow B ( 10) > 6-hydroxykaempferol 3,6-di- O - β - d -glucoside ( 8 ) > hydroxysafflor yellow A ( 3 ) > kaempferol 3- O - β -rutinoside ( 11 ) > 6-hydroxykaempferol 3- O - β -rutinoside ( 9 ) > 6-hydroxykaempferol 3,6-di- O - β - d -glucoside-7- O - β - d -glucuronide ( 4 ) > 6-hydroxyapigenin 6- O - β - d -glucoside-7- O - β - d -glucuronide ( 6 ) > cytidine ( 1 ) > 6-hydroxykaempferol 3- O - β -rutinoside-6- O - β - d -glucoside ( 7 ) > 6-hydroxykaempferol 3,6,7-tri- O - β - d -glucoside ( 5 ) > adenosine ( 2 ). These results demonstrate that quinochalcone C -glycosides ( 3 and 10 ) and some flavonoid glycosides containing C7-OH (such as 8 , 9 and 11 ) made a greater contribution to the overall effect of safflower than the other components that were knocked out. The results provided an important reference for improving quality control and further development of safflower products. And this approach should also be useful for investigating the bioactive constituents of other medicinal herbs. [ABSTRACT FROM AUTHOR]

Buddleoside (also known as linarin) as the major flavonoid in Chrysanthemum morifolium Ramat., has been reported to possess a wide range of pharmacological activities. The human intestinal microbiota might have an important impact on drug metabolism and ultimately on the drug oral bioavailability. However, the interaction of the buddleoside with human intestinal bacteria remains unknown. In this study, the conversion of buddleoside by different bacteria from human feces was firstly investigated. A reliable, sensitive and rapid analytical method, ultra performance liquid chromatography was established and successfully applied to investigate the metabolites and metabolic profile of buddleoside by human intestinal bacteria. Among the isolated bacteria, four strains including Escherichia sp. 4, Escherichia sp. 34, Enterococcus sp. 45 and Bacillus sp. 46 showed more powerful conversion capability. Based on the accurate mass data and the characteristic MS n product ions, the parent and six metabolites were detected and tentatively identified compared with blank samples. The metabolites were produced by four main metabolic pathways including deglycosylation, acetylation, methylation and hydroxylation. Buddleoside could be firstly converted to its aglycon acacetin (M2) by the majority of the isolated intestinal bacteria. Subsequently, M2 was further metabolize to its methylated (M3), acetylated (M4), hydroxylated (M5) and hydrogenated product (M6). However, acacetin-7-glucosid (M1) was obtained only from the minor bacterial samples like Bacillus sp. 46. To further explain the metabolism of buddleoside, the β- d -glucosidase and α- l -rhamnosidase activities of four strains were analyzed. Bacillus sp. 46 could only produce α- l -rhamnosidase, while the other three strains showed two kinds of enzyme activities. Furthermore, the activities of α- l -rhamnosidase and β- d -glucosidase reached the highest level at 12–18 h and 10–12 h, respectively. The metabolic routes and metabolites of buddleoside produced by human intestinal microflora were firstly reported in this paper. The results will be very helpful for the further investigation of the pharmacokinetic research of buddleoside and to unravel how it works in vivo . [ABSTRACT FROM AUTHOR]

Abstract: Ethnopharmacological relevance: Hypericum perforatum (St. John''s wort) is an important anti-depressant herb used in clinic and commonly prescribed for mild depression. Hyperoside is one of the major components of H. perforatum and is also detected in many plant species such as Abelmoschus manihot, Black Currant, Rosa agrestis, Apocynum venetum and Nelumbo nucifera. Aim of the study: As the hyperoside showed CNS (central nervous system) protective activity (e.g. anti-depressant-like effect), the possibility of hyperoside or its metabolites to reach CNS should be investigated. Moreover, the pharmacokinetics profile of hyperoside or its metabolites in rat brain should be studied for further elucidating the mechanism of hyperoside action on CNS. Material and Methods: A simple method for simultaneous determination of unbound hyperoside and its metabolite 3′-O-methyl-hyperoside in rat brain was developed by using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS) and microdialysis technique. This method was applied for pharmacokinetics study of hyperoside and 3′-O-methyl-hyperoside in rat brain after intragastric (i.g.) and intraperitoneally (i.p.) administration of hyperoside in vivo. Results: Results showed that neither hyperoside nor its metabolites were detected in rat brain after i.g. administration but both compounds could be detected after i.p. administration. Considering the activity of hyperoside through both i.g. and i.p. administration, our results imply that the active components of hyperoside in vivo might be different. Therefore, further studies are needed to identify the active components of hyperoside in vivo through these two different routes. Moreover, non-oral administration route (e.g., i.p.) should be further investigated and be explored to obtain higher bioavailability and better activity for hyperoside. Our results also showed that the real existing form of hyperoside in rat brain were hyperoside and its methylated metabolite with maximum concentration to be 63.78ng/mL and 24.66ng/mL after 20mg/kg i.p. administration, respectively. Therefore, a more reasonable concentration of hyperoside should be considered in in vitro assay to reflect the real situation of hyperoside concentration in vivo. Conclusion: Due to the wide use of herbal remedies containing hyperoside, our investigation will contribute to further clarifying the action of this substance. Moreover, this method will be applied for clinical pharmacokinetics study of hyperoside and its metabolite as well as herbs that contain hyperoside. [Copyright &y& Elsevier]

Abstract: Aim of the study: This present study was carried out to evaluate the anti-inflammatory and analgesic effects of 85% ethanol extract (EE) of Commiphora myrrha and its different fractions partitioned with petroleum ether extract (EPE), ethyl acetate extract (EEA), n-butanol extract (EBu), and the water extract (ECY). Moreover, the chemical constituents in EPE were analyzed and identified by UPLC–QTOF/MS/MS. Materials and methods: The anti-inflammatory activities were investigated by utilizing the paw edema mice induced by formalin. In addition, we determined the levels of PGE2 in the edema paw. While the analgesic activity was examined against thermally and chemically induced nociceptive pain in mice, using the acetic acid and hot-plate test methods. The effects of the administration of dolantin or indomethacin were also studied for references. The components in EPE were analyzed by the ultra-performance liquid chromatography coupled with mass spectrum. Results: In the anti-inflammatory test, EE inhibited the development of paw swelling induced by formalin significantly. The pharmacological activities of the petroleum ether fraction (EPE) were stronger than the EE extract and other fractions at the dose of 100mg/kg, and furthermore significantly decreased the levels of inflammatory factor PGE2 in the edema paw tissue at the fourth hour after formalin injection. It has been also shown that the ethanol extract (EE) significantly reduced acetic acid-induced writhing response in mice at the dose of 200mg/kg, and 100mg/kg. The petroleum ether fraction (EPE) showed significant analgesic activity in the model at the dose of 100mg/kg (p <0.01), and the ethyl acetate fraction (EEA) exhibited less analgesic activity (p <0.05). All test samples showed no significant analgesic activity on the hot plate pain threshold in mice. The UPLC–MS/MS chromatogram analysis of EPE stated that EPE contains the ingredients of sesquiterpenes, diterpenes, and diterpenic acids. Moreover, seven main compounds were identified. Conclusion: These data demonstrated that the EE and EPE posses analgesic and anti-inflammatory activities and may support the fact the traditional application of this herb in treating various diseases associated with inflammatory pain. [Copyright &y& Elsevier]