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1.
Article in Chinese | WPRIM | ID: wpr-927917

ABSTRACT

The present study investigated the chemical constituents of Scrophulariae Radix and their antitumor activities in vitro. The compounds in the ethyl acetate extract were separated and purified by conventional column chromatographies(such as silica gel, Sephadex LH-20, and ODS column) and semi-preparative high-performance liquid chromatography(HPLC), and their structures were identified by various spectral techniques such as nuclear magnetic resonance(NMR) and mass spectrometry(MS). Twenty-three compounds were isolated and identified as benzyl-β-D-(3',6'-di-O-acetyl) glucoside(1), 5-O-p-methoxybenzoyl kojic acid(2), 5-O-methoxybenzoyl kojic acid(3), 7-O-methylbenzoyl kojic acid(4), 5-O-benzoyl kojic acid(5), methyl ferulate ethyl ether(6), trans-ferulic acid(7), trans-isoferulic acid(8), trans-caffeic acid(9), trans-caffeic acid methyl ester(10), caffeic acid ethyl ester(11), trans-cinnamic acid(12), trans-p-methoxycinnamic acid(13), trans-p-hydroxycinnamic acid(14), trans-p-hydroxycinnamic acid methyl ester(15), 2-(3,4-dihydroxyphenethyl) alcohol(16),(p-hydroxyphenyl) propanoic acid(17), coniferaldehyde(18), sinapaldehyde(19), benzyl β-primeveroside(20), 5-(hydroxymethyl) furfural(21), furan-2-carboxylic acid(22), and decanedioic acid(23). Among them, compound 1 is a new benzyl glucoside, compounds 2-4 are new pyranone compounds, compound 5 is a new natural product of pyranone. The NMR data of compounds 5 and 6 are reported for the first time. Compounds 6 and 20 were isolated from the Scrophularia plant for the first time. Compounds 8, 11, 14, 16, 18, 19, 22, and 23 were isolated from this plant for the first time. The in vitro cytotoxic activities of these compounds against three tumor cell lines(HepG2, A549, and 4 T1) were evaluated. The results showed that compounds 10 and 15 showed cytotoxic activities against HepG2 cells with IC_(50) values of(19.46±0.48) μmol·L~(-1) and(46.10±1.21) μmol·L~(-1).


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal/chemistry , Mass Spectrometry , Plant Roots/chemistry , Scrophularia/chemistry
2.
Article in Chinese | WPRIM | ID: wpr-879179

ABSTRACT

By establishing the preparation process of Scrophulariaceae Radix reference extract(SRRE) and calibrating it, we discussed its feasibility as a substitute for single reference substance in the quality control of Scrophulariae Radix. The SRREs were prepared by solvent extraction method and chromatographic separation technology, and then calibrated with the reference substances of harpagide, angoroside C and harpagoside. The HPLC content determination method of Scrophulariae Radixl was established with SRREs of the known content and the reference substances of harpagide, angoroside C and harpagoside respectively as the control ones. Then the content of three components in Scrophulariae Radix was determined, and the t-test method was used to compare the results of the two methods. With SRRE as references, harpagide, angoroside C and harpagoside were in a good linear relationship(r≥0.999 8) within each range, and the average recovery rate was 98.55% to 100.6%. The t-test results showed that the P values of two determination methods were 0.493, 0.155 and 0.171 for harpagide, angoroside C and harpagoside respectively, indicating no significant diffe-rence between the two methods of content determination. The SRRE can be used as a substitute for the reference in the quality control of Scrophulariaceae Radix. The SRRE can replace the corresponding reference substance for the quality control of Scrophulariae Radix. The results of this study provide new methods and new ideas for the quality evaluation of Scrophulariae Radix, and provide a scientific basis for the application of reference extracts in the quality research of traditional Chinese medicine.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Quality Control , Scrophularia , Scrophulariaceae
3.
Article in Chinese | WPRIM | ID: wpr-873268

ABSTRACT

The safety of traditional Chinese medicine is affected by many factors, and the influence of exogenous harmful substances has been concerned and become a hot spot in recent years, especially heavy metals, pesticide residues and some other harmful substances. In order to explore the effects of non-soil and non-pesticide treatment on residues of these two harmful substances, the heavy metals and agricultural residues of Lilii Bulbus were detected, and the correlation of the data was analyzed. In this experiment, heavy metals and pesticide residues of Scrophulariae Radix were detected, and correlation analysis was conducted for their data. The mechanism of transport phase was interpreted with statistical moment similarity tool of total fingerprint by supramolecular chemistry theory. A large number of experimental data in this paper showed that heavy metals and pesticide contents in Lilii Bulbus basaltifolia had a positive correlation, which was closely related to supramolecular phenomena. Moreover, the similarity of fingerprints between Lilii Bulbus and Scrophulariae Radix suggested that Lilii Bulbus and Scrophulariae Radixa had a high selectivity in absorption of agricultural residues, which proved that the absorption of pesticides in Lilii Bulbus and Scrophulariae Radix from different habitats had the function of supramolecular imprinting template. It was considered that medicinal plant was a giant complex supramolecule with various levels of " imprinted template" . Heavy metals and agricultural residues were also involved in plant growth, forming an " imprinted template" for the formation of supramolecules between agricultural residues and heavy metals. After heavy metals and agricultural residues formed supramolecules, their liposolubility and permeability changed in varying degrees, and their transport in medicinal plants was promoted. Finally, the heavy metal supramolecules of pesticides were absorbed, distributed, aggregated and accumulated in plants. The purpose of the study was to reveal the mechanism of heavy metal and pesticide supramolecule transport, provide a new direction for the treatment of heavy metals and pesticide residues, and ensure the safety of traditional Chinese medicine.

4.
Article in Chinese | WPRIM | ID: wpr-846531

ABSTRACT

Objective: To explore effects of polysaccharides from Scrophulariae Radix (PFR) on glucolipid metabolism and hepatic insulin signaling pathway in type 2 diabetic rats. Methods: Diabetic rat models were constructed by STZ injection, and randomly divided into five groups: model group, low, medium and high dose groups (80, 160, 320 mg/kg) of PFR, and positive drug group of metformin (200 mg/kg); In addition, ordinary feed rats of the same age were set as normal group; Body weight and survival status, fasting blood glucose (FBG), blood lipid (TC, TG, HDL-C, LDL-C), liver function (ALT, AST), renal function (CREA, BUN), glycosylated hemoglobin (GHb), insulin secretion (FINS), C-peptide, SOD, MDA, CAT, GSH-Px, and other indicators were detected after drug delivery for six weeks; HE staining and oil red O staining were used to evaluate the pathological changes and steatosis of liver in rats; Western blotting was used to detect the changes of hepatic insulin signaling pathway related protein. Results: PFR increased the weight of diabetic rats, improved the metabolic function, reducde the content of FBG, GHb, ALT, AST, CREA, BUN, TC, TG, LDL-C, MDA and increased the content of HDL-C, FINS, C-peptide, SOD, CAT and GSH-Px; Western blotting assay showed that PFR could activate IRS-2/PI3K/Akt signaling pathway and increase the protein levels of PPAR-γ and GLUT-4. Conclusion: PFR could improve glucolipid metabolism in type 2 diabetic rats by regulating the hepatic insulin signaling pathway.

5.
Article in Chinese | WPRIM | ID: wpr-773173

ABSTRACT

The quality constant evaluation method was applied in the grade evaluation of Scrophulariae Radix pieces. Nineteen batches of Scrophulariae Radix were measured for the appearance index. Harpagide and harpagoside were taken as index components for the content determination. The traditional grading standard and the modern quality control index were combined to calculate the quality constant and grade Scrophulariae Radix pieces. The results showed that the quality constants ranged between 156. 75 and 491. 65; according to the percentage mass constants,more than 80% were graded as first-class pieces,50%-80% were graded as second-class pieces,and the rest were graded as third-class pieces. The quality constants of first-class Scrophulariae Radix were >393. 32,that of second-class Scrophulariae Radix was between 245. 83 and 393. 32,and that of third-class Scrophulariae Radix was < 245. 83. The study shows that this method can objectively,reasonably and effectively classify Scrophulariae Radix pieces,and further promote and apply the evaluation method of slice model quality constant to prove the rationality,scientificity and practicability.


Subject(s)
Drugs, Chinese Herbal , Reference Standards , Plant Roots , Chemistry , Quality Control , Scrophularia , Chemistry
6.
Article in Chinese | WPRIM | ID: wpr-851317

ABSTRACT

Objective In order to provide a scientific basis for the grade quality standard criterion of Scrophulariae Radix, a HPLC-DAD method was established to acquire fingerprint and detect the content of multiple components. Methods The chromatographic separate was achieved on Elipse XDB-C18 (250 mm × 4.6 mm, 5 μm) column, with the temperature of 25 ℃, using acetonitrile (A)-0.03% phosphoric acid water (B) as the mobile phase gradient elution, a flow rate of 1.0 mL/min, and the detection wavelength was set at 207 nm for fingerprint, 210 nm for Harpagide, 280 nm for harpagoside, and 264 nm for cinnamic acid. The injection volume was 10 μL. The fingerprints of different grades of Scrophulariae Radix from 30 batches were evaluated with a chromatographic fingerprint similarity evaluation system (version 2012), and the content of harpagide, harpagoside, and cinnamic acid was also determined at the same time. Results There were seven common peaks in the fingerprints, the RSD values of relative retention time were lower than 2.0% and those of relative peak area were quite different, which indicated that the main chemical compounds can exist stably in Scrophulariae Radix with different content. Compared with control, the results of fingerprintsimilarity were presented as follows: 5% under 0.7, 12.5% arranged 0.7 to 0.8, 40% between 0.8 and 0.9, and another 42.5% exceed 0.9, demonstrated that there was qualitative difference in various batches of Scrophulariae Radix. Also, the quantitative analysis of multi-index showed the differences in three main compounds, the content respectively was 0.18%—2.89% in harpagide, 0.01%—0.35% in harpagoside, and 0.01%—0.24% in cinnamic acid. Conclusion Suggestions were provided in the formulation of new grade quality standard, such as adding the fingerprints and multi-index detection of main chemical components based on the original criterion of classification.

7.
Article in Chinese | WPRIM | ID: wpr-851065

ABSTRACT

Objective: To investigate the effects and mechanisms of iridoid glycosides of Scrophulariae Radix (IGRS) via endoplasmic reticulum stress-mediated apoptosis pathway on the primary cortical neurons induced by oxygen glucose deprivation/reperfusion (OGD/R). Methods: Newborn SD rats were performed primary cortical neurons culture. And the primary cortical neurons were pretreated with IGRS (50, 100, and 200 μg/mL) for 24 h, and the in vitro model of oxygen-glucose deprivation/reoxygenation (OGD/R) was applied. The neurons purity and morphology were observed under inverted microscope, the cell viability was detected by MTT assay; the intracellular lactate dehydrogenase (LDH) level and superoxide dismutase (SOD) activity were detected by commercial kit. The apoptotic rate was detected by flow cytometry. The expression of C/EBP homologous protein (CHOP), glucose-regulated protein-78 (GRP78) and Caspase-12 protein were detected by western blotting. Results: The cultured primary cortical neurons were plump with high purity in good condition. Compared with the control group, the primary cortical neurons were retracted and rounded after OGD/R treatment, and the surface of the neurons became rough; The cell viability and SOD activity were significantly decreased; The LDH level and apoptotic rate were evidently increased; The expression of CHOP, Caspase-12, and GRP78 were significantly increased. Compared with the model group, IGRS could relieve neurons damage, increase cell viability and SOD activity, decrease LDH level and apoptotic rate, and down-regulate the expression of CHOP, Caspase-12, and GRP78. Conclusion: IGRS can antagonize the neuronal damage induced by OGD/R in primary cortical neurons, and its mechanism is related to the inhibition of endoplasmic reticulum stress-mediated apoptosis.

8.
Article in Chinese | WPRIM | ID: wpr-851049

ABSTRACT

Objective: To rapidly identify the chemical constituents from the aqueous extract of Scrophulariae Radix by UPLC-LTQ- Orbitrap HRMS combined with cleavage pathways of different chemical constituent cluster. Methods: The analysis was performed on an Acquity UPLC® BEH C18 column (100 mm ×2.1 mm, 1.7 μm). The mobile phase consisted of methanol and 0.1% formic acid aqueous solution was used for gradient elution, with a flow rate of 0.20 mL/min. ESI ion source was applied for mass spectra under positive mode. Results: The cleavage pathways of iridoids and phenylpropanoids were summarized based on mass data of standards. The constituents of the aqueous extract of Scrophulariae Radix were further analyzed by using the mass data and element compositions analysis, and referring with the cleavage pathways, literatures and ClogP value. A total of 61 constituents were identified, including 28 iridoids, 27 phenylpropanoids, and six others. Among them, three acetylangoroside C and methoxylscrophuloside B4 were new compounds, and stegioside III was identified from Scrophulariae Radix for the first time. Conclusion: UPLC-LTQ-Orbitrap HRMS can rapidly and comprehensively characterize the chemical constituents of the aqueous extract of Scrophulariae Radix, which provides a reference for the clarification of efficacy material basis and quality control of Scrophulariae Radix.

9.
Chinese Pharmaceutical Journal ; (24): 741-748, 2019.
Article in Chinese | WPRIM | ID: wpr-858021

ABSTRACT

OBJECTIVE: To analyze the difference of chemical constituents in Scrophulariae Radix from different areas by UFLC-Triple TOF-MS/MS. METHODS: Through analysis of the multistage tandem mass spectra, the characteristic peaks were extracted with mass spectrometry data peak matching, peak alignment, and noise filtering. Principal component analysis (PCA) and orthogonal partial least-squares discriminant analysis (OPLS-DA) were used for data processing. The constituents were identified according to MS accurate mass and MS/MS spectrometry fragmentation information, combined with the software of database search and literature. RESULTS: The chemical constituents in Scrophulariae Radix from different areas were clearly distinguished. Thirty-six chemical constituents were indentified as differential compounds. Among them, there were 11 kinds of common differential chemical constituents, i.e., caffeic acid, aucubin, 5-hydroxymethylfurfural, harpagide, 6-O-methylcatapol, verbascoside, p-coumaric acid, ningpogenin, 6″-O-feruloylharpagide, sibirioside A, and harpagoside. CONCLUSION: This study provides experimental data to reveal the influence of ecological environment and genetic variation on metabolite biosynthesis of Scrophulariae Radix.

10.
Article in Chinese | WPRIM | ID: wpr-851549

ABSTRACT

Objective To identify whole ingredients in Niuhuang Qingwei Pills (NQP) and give primary grade evaluation of NQP. Methods Firstly, microscopic characteristics specified by the statutory standard of NQP were summarized. Then new microscopic identification methods were established for Sennae Folium and Gypsum Fibrosum while new thin layer chromatography (TLC) identification methods were established for Bovis Calculus Artifactus, Borneolum Syntheticum, and Rhei Radix et Rhizoma. In addition, microscopic identification method for Menthae Haplocalycis Herba was improved. In this way, whole-ingredient identification of 17 materials were realized. NQP reference drug was developed and applied as accompanying control in whole-ingredient identification and primary grade evaluation of the samples. Results According to the results of 48 samples from 18 manufactures by primary grade evaluation, 10, 37, and 1 samples were classified as superior, qualified, and unqualified, respectively. Conclusion The proposed methods are accurate, simple, and objective, which offers a more comprehensive approach for quality control of NQP. And the methods provide research strategy and experimental basis for further work on establishment of grade standard.

11.
Article in Chinese | WPRIM | ID: wpr-320868

ABSTRACT

This experiment was performed to establish a qualitative analysis on chemical constituents of Scrophulariae Radix by HPLC-ESI-IT-TOF-MS.The analysis was conducted on a C₁₈ column (Kromasil 100-5, 4.6 mm×250 mm, 5 μm) with 0.1% formic acid-acetonitrile as the mobile phase for gradient elution; ESI ion source was used for mass spectra, and data were collected innegative and positive modes. The results showed that 64 compounds from Scrophulariae Radix had been identified by analyzing negative ion mass data including element composition and by comparing with data from literature. Two new compounds (4-hydroxy-6-O-methylcatalpol and acetylangoroside C) and seventeen known compounds were detected from Scrophulariae Radix for the first time. Seventeen known compounds included twelve iridoid glycosides, three phenylpropanoid glycosides and two other kind compounds. This study will provide chemical basis for elucidation of the effective substance in the Scrophulariae Radix.

12.
Article in Chinese | WPRIM | ID: wpr-258428

ABSTRACT

To establish the suitable modern drying processing parameters for Scrophulariae Radix (SR). With reference to the traditional drying processing method of SR and the characteristics of modern drying equipment, the drying process for SR was simulated as the following three stages: temperature-controlled drying-tempering-temperature-controlled drying. Eighteen batches of SR samples were obtained by the drying methods after the orthogonal design experiment with seven factors namely temperature, wind speed, and target moisture for the first stage, tempering time and temperature, as well as temperature and wind speed for the second stage. UPLC-TQ-MS was applied for determination of nine target compounds including catalpol, harpagide, verbascoside, ferulic acid, angroside-C, aucubin, harpagoside, cinnamic acid and ursolic acid in those dried samples and another 19 batches of SR samples collected from genuine producing area. Principal Component Analysis (PCA) was performed, and total energy consumption was also taken into consideration for analysis and evaluation. Results showed that the optimal drying processing method for SR was as follows: drying temperature of 60 ℃, drying wind speed of 50 Hz, and 50% for target moisture in the first stage; 24 h for tempering time and temperature of 20 ℃ in the second stage; drying temperature of 60 ℃, and drying wind speed of 30 Hz in the third stage. The medicinal materials with optimized modern drying processing method were extremely similar to those collected from genuine producing area in the aspect of both external properties and target compounds, and they were in line with the 2015 version of "Chinese Pharmacopoeia" requirements. In addition, they could help to shorten the drying time and increase the efficiency of primary processing, and thus promote the normalization and standardization of primary drying processing for SR.

13.
Chinese Pharmaceutical Journal ; (24): 274-279, 2016.
Article in Chinese | WPRIM | ID: wpr-859203

ABSTRACT

OBJECTIVE: To establish a QTRAP-UPLC-MS/MS method for simultaneous determination of 10 kinds of nucleosides and nucleobases in Scrophulariae Radix processed by different methods, and investigate the influences of different processing methods on contents of nucleosides and nucleobases. METHODS: The contents of 10 kinds of nucleosides and nucleobases in Scrophulariae Radix processed with different methods were simultaneously determined by QTRAP-UPLC-MS/MS, and TOPSIS analysis was used for comprehensive evaluation of nucleosides and nucleobases. RESULTS: The contents of guanosine, uridine, adenosine and uracil were relatively high in Scrophulariae Radix. There were differences in contents of nucleosides and nucleobases of Scrophulariae Radix processed with different methods, and the samples processed by method of "sweating" had better quality. CONCLUSION: This study provides a scientific basis for investigation on the influence of processing methods on contents of nucleosides and nucleobases in Scrophulariae Radix and screening of suitable processing method for Scrophulariae Radix.

14.
Chinese Pharmaceutical Journal ; (24): 1416-1422, 2016.
Article in Chinese | WPRIM | ID: wpr-859010

ABSTRACT

OBJECTIVE: To develop a method for the determination of iridoid, phenylpropanoid glycosides, and organic acids in Scrophulariae Radix from different habitats and commercial herbs by UPLC-QTRAP-MS/MS. METHODS: The analysis was carried out on a BDS HYPERSIL C18 column (4.6 mm×250 mm, 5 μm) with elution by mobile phase of acetonitrile-water at a flow rate of 1.0 mL·min-1. The column temperature was maintained at 35℃. The target compounds were analyzed by the negative ion multiple reaction monitoring (MRM) mode. RESULTS: Twelve multiple constituents showed good linearity (r>0.9994) in the range of the tested concentration. The average recoveries of the 12 components were 99.59%-101.24% with relative standard deviations of 0.93%-1.60%. CONCLUSION: The established method is accurate and precise, which provides a reliable and effective technique for the quality evaluation of Scrophulariae Radix.

15.
Article in Chinese | WPRIM | ID: wpr-447320

ABSTRACT

Objective To construct a simultaneous HPLC-UV dual wavelength spectrometry method for detecting three main contents - harpagide, harpagoside and cinnamic acid in Scrophulariae Radix dispensing particles. Methods Ultimate AQ-C18 column (250 mm×4.6 mm, 5μm) was used, with 1%acetic acid solution and acetonitrile as mobile phase of gradient elution. The flow rate was 1.0 mL/min, detection wavelength was 210 nm at former 13 min and 278 nm after 13 min. The column temperature was 30 ℃. Results The linear range of harpagide, harpagoside and cinnamic acid was 0.066 54-0.665 4 μg (r=1.000 0), 0.024 23-0.242 3 μg (r=0.999 9), and 0.100 28-1.002 8 μg (r=0.999 9), respectively. The average recovery (n=6) was 99.80%±1.22%, 100.31%±1.30% and 100.22%±1.24%, respectively. Conclusion The method is simple, repeatable, stable, and can be used for quality control and standardization of Scrophulariae Radix dispensing particles.

16.
Chinese Pharmaceutical Journal ; (24): 1581-1584, 2012.
Article in Chinese | WPRIM | ID: wpr-860611

ABSTRACT

OBJECTIVE: To investigate the feasibility of using mid-infrared spectroscopy (MIRS) technology for rapid quantification of harpagoside contents in crude and processed Radix Scrophulariae by means of attenuated total reflectance. METHODS: HPLC was used as the reference method to determine the content of harpagoside, and multivariate calibration models based on PLS algorithm were developed to correlate the spectra and the corresponding values determined by the reference method. RESULTS: The determination coefficient of the calibration model for crude Radix Scrophulariae was r2 = 83.81, and the standard error of estimate (SEE) and the standard error of prediction (SEP) were 0.02155 and 0.05103, respectively. The determination coefficient of the calibration model for processed Radix Scrophulariae was r2 = 95.56, and the standard error of estimate (SEE) and the standard error of prediction (SEP) were 0.00730 and 0.03478, respectively. CONCLUSION: The proposed method is fast and nondestructive, and it provides a novel efficient and environmental friendly approach for the fast determination of the active components in crude and processed traditional Chinese medicine (TCM). Copyright 2012 by the Chinese Pharmaceutical Association.

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