Glycyrrhiza inflata Bat. produces a lot of licorice waste after water extraction, which also retains abundant total flavonoids (TFs) and licochalcone A. However, licorice residue is often wasted due to the lack of good utilization of resources in practical applications. This study first screened the optimal membrane pore size and resin type and then explored the mechanism and conditions of the adsorption of TFs on the resin. Then, different combinations and sequences of membrane and macroporous resin (MR) methods were investigated. It was found that using the membrane method for initial purification, followed by the MR method for further purification, yielded the best purification results. Next, response surface methodology was utilized to investigate the resin\'s dynamic desorption conditions for TFs. Finally, the TF purity increased from 32.9% to 78.2% (2.38-fold) after purification by a combined membrane-MR process; the purity of licochalcone A increased from 11.63 mg·g-1 to 22.70 mg·g-1 (1.95-fold). This study verified the feasibility of enriching TFs and licochalcone A from licorice residue using a membrane-MR coupling method. In addition, a quality-control method was established using a fingerprinting method on the basis of ultrahigh-performance liquid chromatography (UPLC) to ensure the stability of the enrichment process.

In this study, thirty-four samples of Laggera crispata (Vahl) Hepper & J. R. I. Wood from five main production areas in Yunnan Province, were collected for experimentation. UPLC- PDA was used to generate fingerprints and the common peaks were analysed through R and SIMCA-P. L. crispata from different origins can be distinguished by OPLS-DA and PCA. The VIP values were compared, and 8 characteristic components with great differences were obtained. It was confirmed that the two characteristic components were chrysosplenetin and artemisetin, and the quantitative analysis was performed with these two compounds from L. crispata samples with different origins. Based on the variance analysis results, the most significant difference in the content of chrysosplendin and artemisin was in Lancang and Honghe and Lancang and Simao, respectively. The chrysosplenetin can be used as an important indicator for quality control and to trace the origin of L. crispata.

Cyclocarya paliurus is an edible and medicinal plant exhibiting significant hypoglycemic effect. However, its active components are still unclear and need further elucidation. In this research, the active components of the leaves of C. paliurus responsible for the α-glucosidase inhibitory activity were screened and identified based on a spectrum-effect relationship study in combination with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) analysis. The 70% ethanol eluate fraction of the leaves of C. paliurus with the strongest α-glucosidase inhibitory activity was obtained after extraction and purification with macroporous resin. Their chromatographic fingerprints (15 batches) were established by UPLC analysis and 32 common peaks were specified by similarity analysis. Their IC50 values for α-glucosidase inhibition were measured by an enzymatic reaction. Several multivariate statistical analysis methods including hierarchical cluster analysis, principal component analysis, partial least square analysis and gray relational analysis were applied to explore the spectrum-effect relationship between common peaks and IC50 values, and the chromatographic peaks making a large contribution to efficacy were screened out. To further elucidate the active components of leaves of C. paliurus, the 70% ethanol eluate fraction was characterized by UPLC-MS/MS analysis, and 10 compounds were identified. This study provides a valuable reference for further research and development of hypoglycemic active components of C. paliurus.

Twenty batches of Aurantii Fructus Immaturus(AFI) were collected, with their peel and pulp taken as research objects. Ultra-high performance liquid chromatography(UPLC) fingerprints of peel and pulp of AFI were established with 17 common peaks in peel and 10 in pulp. Six kinds of flavonoids were identified, i.e., narirutin, naringin, rhoifolin, hesperidin, neohesperidin and nobiletin. The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine was employed for similarity analysis, which showed that the chromatographic peaks of peel and pulp were basically similar to their respective reference fingerprints, with all similarities greater than 0.90. The similarity between peel and pulp of the same batch of AFI ranged from 0.850 to 0.983. Cluster analysis(CA), principal component analysis(PCA), and orthogonal partial least squares discriminant analysis(OPLS-DA) were conducted on the common peaks of peel and pulp of AFI with SPSS 17.0 and SIMCA 14.1. Combined with the reference fingerprints, these analyses revealed 12 differential components regarding peel and pulp. Further, the content of the 6 flavonoids and synephrine was determined. The proposed method integrating UPLC fingerprint and multicomponent quantitative analysis is applicable to the quality evaluation of AFI. The results provide a certain basis for the scientific connotation about the appearance characteristic of AFI.

Zhishi-Xiebai-Guizhi Decoction (ZSXBGZD), a traditional Chinese medicine (TCM) formula, has been used for treatment of coronary heart disease and myocardial infarction for nearly two thousand years. However, the chemical composition of ZSXBGZD is still unclear. In order to obtain the chemical profile of ZSXBGZD, an ultra-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) method was utilized for the identification of its multi-constituents. As a result, a total of 148 compounds were identified based on their retention times, accurate masses and MS/MS data. In addition, an optimized UPLC fingerprint analysis, combined with chemometrics such as similarity analysis (SA), hierarchical cluster analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) was developed for quality assessment of ZSXBGZD. Multivariate data analysis revealed that samples could be classified correctly according to their geographic origins, and four compounds neohesperidin, naringin, guanosine and adenosine contributed the most to classification. The established UPLC method with multi-wavelength detection was further validated and implemented for simultaneous quantification of 12 representative ingredients in the prescription, including guanosine, adenosine, 2\'-deoxyadenoside, syringin, magnoloside A, forsythoside A, naringin, hesperidin, cinnamaldehyde, neohesperidin, honokiol and magnolol. This is the first report on the comprehensive profiling of major chemical components in ZSXBGZD. The results of the study could help to uncover the chemical basis of ZSXBGZD and possess potential value for quality evaluation purpose.

To establish ultra performance liquid chromatography( UPLC) fingerprint of Puerariae Lobatae Radix from different habitats and simultaneously determine the contents of six isoflavonoids. The UPLC fingerprint analysis and content determination were performed on a Waters ACQUITY UPLC BEH C_(18)( 2. 1 mm×50 mm,1. 7 μm) chromatographic column,with acetonitrile-0. 05% formic acid as mobile phase for gradient elution. The detection wavelength was set at 250 nm; the flow rate was 0. 2 mL·min~(-1); the column temperature was 30 ℃ and the injection volume was 2 μL. Similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine( TCM) was adopted; principal component analysis( PCA) and discriminant analysis by partial least square method( PLS-DA) in Simca-P software were used to identify the differential components in samples from three habitats. The similarity was over 0. 90 in 29 batches of samples,indicating good consistency of the samples. The samples were clustered into 3 categories by PCA and PLS-DA,and six differential components such as puerarin apioside,daidzin,and isoflavoues aglycone were found. The determination results of 6 isoflavones,including 3\'-hydroxy puerarin,puerarin,3\'-methoxy puerarin,puerarin apioside,daidzin,and isoflavoues aglycone,showed that the content of the same component and the fluctuation range between different components were all different among different habitats. The total content of 6 isoflavones from different regions was Anhui 11. 21% >Henan 10. 97% >Shannxi 9. 38%. The establishment of UPLC fingerprint combined with simultaneous determination of 6 active components provides a more comprehensive reference for quality control and quality evaluation of Puerariae Lobatae Radix.

BACKGROUND: Codonopsis Radix is a commonly used traditional Chinese medicine, and has the effect of strengthening spleen and tonifying lung, nourishing blood and engendering liquid. In addition, it is also used as important food materials.
OBJECTIVE: The aim of the study was to explain the underlying correlations between chemical constituents and pharmacological effects and explore the bioactive markers of Codonopsis Radix.
METHODS: Codonopsis Radix samples from Min county, Gansu province processed with different methods were taken as the materials, UPLC-ESI-Q-TOF-MS/MS analysis was conducted to identify the compounds and establish UPLC fingerprint. Meanwhile, hematopoietic and immunologic functions of Codonopsis Radix were investigated to obtain relevant pharmacological index. Then, the correlation analysis between chemical constituents in UPLC fingerprints and pharmacological effects was carried out. The plant name was confirmed to the database \"The Plant List\" (www.theplantlist.org).
RESULTS: According to the results of canonical correlation analysis, tryptophan, syringin, tangshenoside I, codonopyrrolidium A, lobetyolin and two unknown compounds might be the potential bioactive markers related to the hematopoietic and immunologic functions of Codonopsis Radix, which could be recommended as the index compounds.
CONCLUSIONS: This study illustrated the underlying correlations between chemical constituents and pharmacological effects, explored the pharmacological material basis, and could lay a foundation for the improvement of quality standard of Codonopsis Radix.

To establish a content determination method for 2,3,5,4\'-tetrahydroxy stilbene-2-O-β-D-glucoside (TSG) of the crude/processed root of Polygonum multiflorum from different habitats in China and set up the fingerprint by using UPLC. Various samples were pretreated by macro-porous resin. Then UPLC analysis was performed on Waters ACQUITY UPLC@BEH C18 chromatographic column (2.1 mm×50 mm, 1.7 μm) at (25±5) ℃. A binary gradient elution system was composed of acetonitrile (phase A) and 0.5% acetic acid solution (phase B). Detection was performed at the wavelength of 254 nm, and the mobile flow rate was set at 0.3 mL•min⁻¹. Results showed that the yield of extraction of the 2,3,5,4\'-tetrahydroxy stilbene-2-O-β-D-glucoside from root of P. multiflorum was all over 25.0% after macro-porous resin separation; an exclusive UPLC fingerprint method of the crude/processed root of P. multiflorum from different habitats was successfully set up and 17 chromatographic peaks were calibrated. Cluster analysis can not entirely distinguish the crude one from the processed one, while principal component analysis absolutely can. 2,3,5,4\'-tetrahydroxy stilbene-2-O-β-D-glucoside is the composition that has largest differences in variable importance in projection (VIP) between crude and processed root of P. multiflorum. The separating method can gain high-purity 2,3,5,4\'-tetrahydroxy stilbene-2-O-β-D-glucoside, and the determination method is simple, sensitive, reliable and can be used in fast identifying the crude/processed root of P. multiflorum or as a method for overall quality control of root of P. multiflorum.

Evodia rutaecarpa (E. rutaecarpa) has been used to treat aches, vomiting and dysentery in traditional Chinese medicine. However, as a mildly toxic herb its toxic components have not been elucidated. An attempt was made to illuminate the hepatotoxic constituents of E. rutaecarpa. The 50% ethanol extracts of E. rutaecarpa from 19 different sources were used to establish UPLC fingerprints and administered to mice at a dose of 35 g/kg (crude medicine weight/mouse weight) once daily for 14 days. Serum levels of alanine transaminase, aspartate aminotransferase and liver coefficient were used as indices of liver injury. Additionally, the characteristic peaks of 19 fingerprints were identified. Spectrum-effect relationships between fingerprints and hepatotoxic indicators were analyzed using bivariate correlation analysis (BCA). The UPLC fingerprints were established and a total of 28 main compounds were identified. Because of the inherent variations in chemical compositions, the liver injury levels were different among the E. rutaecarpa samples from 19 sites of production. BCA results indicated that compounds dihydrorutaecarpine, 6-acetoxy-5-epilimonin, goshuyuamide I, 1-methyl-2-[(Z)-5-undecenyl]-4(1H)-quinolone, 1-methyl-2-[(4Z,7Z)-4,7-tridecadienyl]-4(1H)-quinolone, evocarpine and 1-methyl-2-[(6Z,9Z)-6,9-pentadecadienyl]-4(1H)-quinolone were tentatively determined as the primary hepatotoxic components. The present study provides a valuable method for the discovery of hepatotoxic constituents by combination of fingerprints and hepatotoxicity index.