Xin Chai

Characterization and quantification of major constituents of Xue Fu Zhu Yu by UPLC-DAD-MS/MS.

Xue Fu Zhu Yu (XFZY), a classic recipe in traditional Chinese medicine (TCM), has been demonstrated to show protective effects on cardiovascular system. For quality control of XFZY products, qualitative analysis using ultra high performance liquid chromatography with diode-array detector-tandem mass spectrometry (UPLC-DAD-MS) was undertaken. Twenty-eight compounds from XFZY were simultaneously detected; among them, seventeen compounds were unequivocally identified, and another eight compounds were tentatively characterized. According to qualitative results, a new method for quantitative analysis of XFZY has been established by ultra high performance liquid chromatography coupled with diode array detector (UPLC-DAD). Twelve representative compounds unequivocally identified were used as chemical markers in quantitative analysis, including 5-hydroxymethyl-2-furaldehyde (5-HMF), hydroxysafflor yellow A (HSYA), amygdalin, albiflorin, paeoniflorin, liquiritin, ferulic acid (FA), naringin, hesperidin, neohesperidin (NH), isoliquiritigenin (IL) and glycyrrhizic acid (GA), which were derived from nine of eleven herbs of XFZY except Platycodon grandiflorum (Jacq.) A. DC. (Jiegeng) and Bupleurum chinense DC. (Chaihu). This UPLC method was validated in terms of linearity, LOD and LOQ, precision, repeatability, stability, and recovery tests. Quality control of XFZY products in total fourteen samples by four dosage forms was examined by this method, and results confirmed its feasibility and reliability in practice.

A rapid ultra performance liquid chromatography–tandem mass spectrometric method for the qualitative and quantitative analysis of ten compounds in Eucommia ulmodies Oliv.

A rapid method for qualitative and quantitative analysis of constituents in Eucommia ulmoides Oliv. was developed by ultra performance liquid chromatography with electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS). Ten compounds including iridoids, phenylpropanoids, and flavonoids were identified and further quantified as marker substances by UPLC-UV using switching UV wavelength within 16min. The separation was carried out on an Acquity UPLC BEH C(18) column with 0.1% formic acid aqueous solution and acetonitrile as the mobile phase under gradient conditions. The developed method was applied to the quality assessment of various E. ulmoides samples, including different medicinal parts, differently processed bark and bark from different habitats. The results showed that the branches of E. ulmoides were not suitable for medicinal use. The process of carbonizing led to significant loss of major components, whereas the process of stir-frying with salt-water enhanced the extraction of chlorogenic acid with negligible loss of the other components. The contents of the investigated compounds varied very remarkably for the bark of E. ulmoides collected from different habitats. This study might provide a comprehensive method for the quality assessment of E. ulmoides.

Chemical material basis study of Xuefu Zhuyu decoction by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

Xuefu Zhuyu decoction, a classic prescription in traditional Chinese medicine, has been widely used in the clinical treatment of cardiovascular and cerebrovascular diseases. In order to profile the chemical material basis of this formula, an ultra-performance liquid chromatography (UPLC) coupled with quadrupole time-of-flight mass spectrometry (Q/TOF MS) method has been established for rapid separation and structural characterization of compounds in the decoction. As a result, 103 compounds including phenolic acids, spermidines, C-glycosyl quinochalcones, terpenoids, flavonoids, saponins, and others were detected; 35 of them were unambiguously identified, and 68 were tentatively characterized by comparing the retention time, MS data, characteristic MS fragmentation pattern and retrieving the literature. In conclusion, the UPLC coupled with quadrupole time-of-flight mass spectrometry method developed in this work is an efficient approach to perform chemical material basis studies of traditional Chinese medicine formulae.

Sensitive and Simplified Detection of Antibiotic Influence on the Dynamic and Versatile Changes of Fecal Short-Chain Fatty Acids.

Short-chain fatty acids (SCFAs), produced by anaerobic fermentation of mainly indigestible dietary carbohydrates by gut microbiota, have a profound influence on intestinal function and host energy metabolism. Antibiotics may seriously disturb the balance of fecal SCFAs. To evaluate the impacts of antibiotics on fecal SCFAs produced by gut microbiota, a simple, reproducible and accurate gas chromatography (GC) method, which can simultaneously analyze seven SCFAs in fecal samples, was developed and validated. The ranges of detection and quantitation of the SCFAs reached 0.0868 ~ 0.393 and 0.261 ~ 1.18 μg·mL-1 respectively, in an optimized protocol for SCFAs extraction and analysis that used 10 mL 75% ethanol aqueous solution containing 1% HCl, without ultrasonication. The technique exhibited excellent intra-day (relative standard deviation (RSD) ≤ 2.54%) and inter-day (RSD ≤ 4.33%) precisions for all the SCFAs. Later, we administered broad-spectrum antibiotics, cefdinir or azithromycin to rats and analyzed the alterations in fecal SCFAs. The total amount, types and distribution of nearly all fecal SCFAs were significantly altered during the administration and even after withdrawal of the antibiotics in rats. The effects of cefdinir on the SCFAs were more pronounced than those of azithromycin. Our findings suggest SCFAs may serve as sensitive indicators to monitor the influences of antibiotics on SCFAs originated by intestinal bacteria. Our improved SCFAs analysis method is a potential platform for a standard clinical test of the effects of new antibiotics on SCFAs.

Phytochemical and Pharmacological Studies on the Genus Psoralea: A Mini Review

The genus Psoralea, which belongs to the family Fabaceae, comprises ca. 130 species distributed all over the world, and some of the plants are used as folk medicine to treat various diseases. Psoralea corylifolia is a typical example, whose seeds have been widely used in many traditional Chinese medicine formulas for the treatment of various diseases such as leucoderma and other skin diseases, cardiovascular diseases, nephritis, osteoporosis, and cancer. So, the chemical and pharmacological studies on this genus were performed in the past decades. Here, we give a mini review on this genus about its phytochemical and pharmacological studies from 1910 to 2015.

Dose-dependent targeted knockout methodology combined with deep structure elucidation strategies for Chinese licorice chemical profiling.

One of the limitations with regards to the chemical profiling of Chinese herbs is that low-level compounds are masked by high-level structures. Here, we established a novel methodology based on a dose-dependent targeted knockout (DDTK) technique combined with deep structure elucidation strategies to allow the chemical profiling of Chinese licorice. We employed ultra-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q/TOF MS) incorporated with the DDTK technique to identify the compounds in different concentration samples and found that the compounds at the high- or medium-level were detected readily in the sample at a low concentration; subsequently, minor or trace-level constituents were identified in the sample at a high concentration by rejecting high-level constituents detected in the sample at a low concentration based on a heart-cutting technique during analysis. In this study, among the 232 compounds detected, 27 compounds were unequivocally identified and 165 compounds, including 29 new compounds and two new natural products, were tentatively characterized. The novel methodology established in this work paves the way the further identification of compounds from complicated mixtures, especially traditional Chinese medicines.

Quality Evaluation of Astragali Radix Products by Quantitative Analysis of Multi-components by Single Marker

Abstract Objective To develop a quantitative analysis of multi-components by single-marker (QAMS) method for the simultaneous determination of eight components in Astragali Radix products, and to examine the feasibility of using the method among the different dosage forms and between two different types of compounds. Methods Eight main effective components, campanulin, genistin, ononin, calycosin, genistein, formononetin, methylnissolin, and astragaloside IV were selected as analytes for the quality control of Astragali Radix products. Calycosin was selected as the internal reference substance, the content of which was determined by external standard method; the relative correction factors (RCFs) of campanulin, genistin, ononin, genistein, formononetin, methylnissolin, and astragaloside IV were calculated. In total, twelve Astragali Radix specimen in decoction pieces, as well as in two different dosage forms, such as granule and oral liquid products, were used for the quality control by both methods of external standard and QAMS. The validity of the QAMS method was evaluated by comparison on the quantitative results of the two methods. Results These RCFs were obtained with good reproducibility (RSD Astragali Radix products determined by the two methods. Conclusion QAMS is a reliable and feasible method in determining the components in products of Astragali Radix.

Characteristic chromatographic fingerprint study of short-chain fatty acids in human milk, infant formula, pure milk and fermented milk by gas chromatography–mass spectrometry

Abstract Human milk, infant formula, pure milk and fermented milk as food products or dietary supplements provide a range of nutrients required to both infants and adults. Recently, a growing body of evidence has revealed the beneficial roles of short-chain fatty acids (SCFAs), a subset of fatty acids produced from the fermentation of dietary fibers by gut microbiota. The objective of this study was to establish a chromatographic fingerprint technique to investigate SCFAs in human milk and dairy products by gas chromatography coupled with mass spectrometry. The multivariate method for principal component analysis assessed differences between milk types. Human milk, infant formula, pure milk and fermented milk were grouped independently, mainly because of differences in formic acid, acetic acid, propionic acid and hexanoic acid levels. This method will be important for the assessment of SCFAs in human milk and various dairy products.

Establishment of a ternary network system for evaluating the antioxidant fraction of Danhong injection

Oxidative stress plays a crucial role in numerous cardiovascular diseases. As an effective therapy, Danhong injection (DHI) is considered to act through an antioxidant mechanism for the treatment of cardiovascular disease. In our study, we focused on the potential contribution of the antioxidant capacity of DHI fractions (Frs) and established an innovative screening method based on a 2,2-diphenyl-1-picrylhydrazyl radical scavenging activity assay. A ternary network evaluation system, which was constructed based on the radical scavenging activity, the area under the activity-concentration curve and the solid content of the fractions, was implemented to select the fractions that posed the greatest antioxidant effect. As a result, Frs 5-7 and Frs 17-19 were shown to exhibit superior antioxidant activity according to the regression area of the ternary network, which was >0.5. Furthermore, the active fractions were characterized by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry combined with nuclear magnetic resonance. This study provided an effective method for the comprehensive evaluation of the antioxidant effect of DHI fractions. Copyright

A new caffeoylgluconic acid derivative from the nearly ripe fruits of Evodia rutaecarpa

A new caffeoylgluconic acid derivative, trans-caffeoyl-6-O-d-gluconic acid methyl ester (1), together with two known compounds named trans-caffeoyl-6-O-d-glucono-γ-lactone (2) and trans-caffeoyl-6-O-d-gluconic acid (3), was isolated from the nearly ripe fruits of Evodia rutaecarpa (Juss.) Benth.. These compounds were isolated by various separation methods associated with the UPLC-Q-TOF-MS technique. Their structures were elucidated on the basis of extensive spectroscopic methods.