1.Correlations between appearance traits and internal quality of Bupleurum scorzonerifolium roots based on theory of "quality evaluation through morphological identification".
Wen-Xue WANG ; Xiao-Wei DU ; Bing-Yan HOU ; Hong-Ru ZHU ; Dan YU
China Journal of Chinese Materia Medica 2023;48(7):1815-1823
It is generally believed that high-quality Bupleurum scorzonerifolium roots possess specific morphological characteristics, being red, robust, and long with strong odor. However, the scientific connotation of these characteristics has not been elucidated. According to the theory of "quality evaluation through morphological identification", we studied the correlations between appearance traits(the RGB value of root surface, root length, root diameter, dry weight, and ratio of phloem to xylem) and content of main chemical components(volatile oils, total saponins, total flavonoids, total polysaccharides, and seven saikosaponins) of B. scorzonerifolium roots. Epson Scanner and ImageJ were used to scan the root samples and measure the appearance traits. Ultraviolet spectrophotometry and HPLC were employed to determine the content of chemical components. The correlation, regression, and cluster analyses were performed to study the correlations between the appearance traits and the content of chemical components. The results showed that the content of volatile oils and saikosaponins were significantly correlated with RGB value, root length, and root diameter, indicating that within a certain range, the roots being redder, longer, and thicker had higher content of volatile oils and saikosaponins. According to the appearance traits and chemical component content, the 14 samples from different producing areas were classified into four grades, and the differences in morphological traits and chemical component content were consistent among different grades. The findings in this study demonstrate that appearance traits(RGB value, root length, and root diameter) can be used to evaluate the quality of B. scorzonerifolium roots. Meanwhile, this study lays a foundation for establishing an objective quality evaluation method for B. scorzonerifolium roots.
Bupleurum/chemistry*
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Saponins/analysis*
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Oleanolic Acid/analysis*
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Oils, Volatile/analysis*
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Plant Roots/chemistry*
2.Simultaneous determination and pharmacokinetic study of five compounds from total extract of Clinopodium chinense in abnormal uterine bleeding rat plasma by UPLC-MS/MS.
Li-Li LI ; Qi HUANG ; Jia-Jia QI ; Min YAO ; Dai-Yin PENG
China Journal of Chinese Materia Medica 2022;47(18):5071-5078
Clinopodium chinense, a traditional folk medicinal herb, has been used to treat abnormal uterine bleeding(AUB) for many years. Saponins and flavonoids are the main active components in C. chinense. To study the pharmacokine-tics of multiple components from the total extract of C. chinense(TEC), we established a sensitive and rapid method of ultra-perfor-mance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS) for simultaneous determination of five compounds in the plasma of AUB rats. After validation, the AUB model was established with SD female rats which got pregnant on the same day by gavage with mifepristone(12.4 mg·kg~(-1)) and misoprostol(130 μg·kg~(-1)). The established method was applied to the detection of hesperidin, naringenin, apigenin, saikosaponin a, and buddlejasaponin Ⅳb in AUB rats after the administration of TEC. The pharmacokinetic parameters were calculated by DAS 2.0. The five compounds showed good linear relationship within the detection range. The specificity, accuracy, precision, recovery, matrix effect, and stability of the method all matched the requirements of biolo-gical sample detection. The above 5 compounds were detected in the plasma of AUB rats after the administration of TEC. The C_(max) va-lues of hesperidin, naringenin, apigenin, saikosaponin a, and clinoposide A were 701.6, 429.5, 860.7, 75.1, and 304.1 ng·mL~(-1), respectively. All the compounds owned short half-life and quick elimination rate in vivo, and the large apparent volume of distribution indicated that they were widely distributed in tissues. Being rapid, accurate, and sensitive, this method is suitable for the pharmacokinetic study of extracts of Chinese herbal medicines and provides a reference for the study of pharmacodynamic material basis of C. chinense in treating AUB.
Administration, Oral
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Animals
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Apigenin/analysis*
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Chromatography, High Pressure Liquid/methods*
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Chromatography, Liquid
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Drugs, Chinese Herbal/chemistry*
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Female
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Flavonoids/analysis*
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Hesperidin
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Lamiaceae
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Mifepristone
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Misoprostol
;
Oleanolic Acid/analogs & derivatives*
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Plant Extracts/chemistry*
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Rats
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Saponins
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Tandem Mass Spectrometry/methods*
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Uterine Hemorrhage
3.Determination of oleanic acid and paeoniflorin in Paeonia lactiflora by ultrasound-assisted ionic liquid-reversed phase liquid chromatography.
Wei LIU ; Dong-dong LI ; Hong-shuai YANG ; Yuan-yuan CHEN ; Jin-feng WEI ; Wen-yi KANG ; Xiu-chun GUO
China Journal of Chinese Materia Medica 2015;40(3):443-449
Four kinds of ionic liquids [BMIM] Br, [BMIM] BF4, [BMIM] PF6, [HMIM] PF6 were used to analyze the content of oleanic acid and paeoniflorin in Paeonia lactiflora with ultrasonic-assisted extraction coupled with HPLC. The chromatographic column, Purospher star RP-C18 (4.6 mm x 250 mm, 5 μm), was used. Acetonitrile and water (90:10) as mobile phase was used to determine the content of oleanic acid with a gradient elution and flow rate at 1.00 mL · min(-1), detection wavelength at 210 nm, chromatographic column temperature at room temperature. Paeoniflorin content was determined using acetonitrile and water (18:82) as mobile phase with a gradient elution and flow rate at 1.00 mL · min(-1), detection wavelength at 250 nm, the chromatographic column temperature at room temperature. The result show that oleanic acid has the highest extraction yield when the conditions are solid-liquid ratio of 1:80 (g · mL(-1)), and the [BMIM] Br methanol solution concentration of 0.6 mol · L(-1). Under the optimal extraction conditions, the content of oleanic acid from 0.24 to 3.76 μg showed a good linearity (r = 0.9999), the average recovery was 97.20%. Paeoniflorin has the highest extraction yield when the conditions are solid-liquid ratio of 1:130 (g · mL(-1)), and the [C4 MIM] PF6 methanol solution concentration of 0.6 mol · L(-1). Under the optimal extraction conditions, paeoniflorin content from 0.42 to 4.20 μg showed a good lin- earity (r = 1.000), the average recovery was 98.84%. This method is simple and reliable, its repeatability is also very good. It has important significance in the study P. lactiflora of ionic liquid microextraction.
Chromatography, Reverse-Phase
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methods
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Glucosides
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analysis
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Ionic Liquids
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chemistry
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Monoterpenes
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analysis
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Oleanolic Acid
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analysis
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Paeonia
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chemistry
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Ultrasonics
4.Establishment of quality standard for Corni Fructus based on the multiple bioactive constituents.
Sheng GUO ; Jin-ao DUAN ; Shao-qing ZHU ; Da-wei QIAN
China Journal of Chinese Materia Medica 2015;40(15):3017-3021
This study is to establish the methods for determination of iridoid glycosides and triterpenic acids in Corni Fructus and provide technical support for the quality control of Corni Fructus. Morroniside, loganin and sweroside were determined by HPLC-UV method with acetonitrile and 0.1% formic acid as the mobile phase, and the detective wavelength was set at 240 nm. Oleanolic acid and ursolic acid were determined by HPLC-ELSD method with methanol-0.5% ammonium acetate (87:13) as the mobile phase. The results showed that the linear ranges of morroniside, loganin and sweroside were 5.335-213.4 mg · L(-1) (r = 0.9999), 5.515-220.6 mg · L(-1) (r = 1.0000), 1.992-79.68 mg · L(-1) (r = 1.0000), respectively. The average recoveries of the above three iridoid glycosides were 98.49%-99.28% with RSDs of recoveries being less than 2%. The linear ranges of oleanolic acid and ursolic acid were 7.74-154.8 mg · L(-1) (r = 0.9964), 10.82-216.4 mg · L(-1) (r = 0.9996), respectively. The average recoveries of the above two triterpenic acids were 98.11%-99.27% with RSDs of recoveries being less than 3%. The method established in this research is simple, rapid and reliable, and can be used for quality control of Corni Fructus. Furthermore, the research provided experimental data for the improvement of present quality standard of Corni Fructus, which has important significance to guarantee its quality and clinical curative effect.
Cornus
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chemistry
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Drug Stability
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Oleanolic Acid
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analysis
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Quality Control
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Triterpenes
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analysis
5.Research on quality standards of zhuang medicine Lonicerae dasystylae flos.
Rui-Song HUANG ; Zheng-Lin LU ; Dong-Jie QIN ; Yue-Kui LIAO ; Zi-Ning LIANG
China Journal of Chinese Materia Medica 2013;38(5):762-767
OBJECTIVETo establish quality standard of Zhuang medicine Lonicera dasystyla, and provide scientific basis for the quality control of L. dasystyla.
METHODCharacteristics of materia medica, microscopic features, TLC indentification, inspection, extractum and determination of chlorogenic acid, macranthoidin B, dipsacoside B were carried out through the experience, microscopic, physical and chemical methods, respectively. The standard of quality control was formulated thereafter.
RESULTThe characteristics of materia medica, microscopic features, TLC indentification were specified, the average contents of water, total ash, acid-insoluble ash, alcohol-soluble extracts, chlorogenic acid were 11.6%, 6.6%, 0.2% , 24.4%, 1.16%, respectively, the total amount of macranthoidin B and dipsacoside B was 3.13%. Quality standard of L. dasystyla was proposed according to experimental results.
CONCLUSIONThe quality of L. dasystyla can be controlled effectively with the quality standard.
Chlorogenic Acid ; analysis ; isolation & purification ; Chromatography, Thin Layer ; Drugs, Chinese Herbal ; chemistry ; standards ; Lonicera ; chemistry ; Oleanolic Acid ; analogs & derivatives ; analysis ; isolation & purification ; Quality Control ; Saponins ; analysis ; isolation & purification ; Solubility
6.Study on TLC identification of Dida commonly used in Tibetan medicine from different species.
Yong YANG ; Guo-Yue ZHONG ; Xiao-Yun WU ; Wei-Zao LUO ; Dan-Dan GU
China Journal of Chinese Materia Medica 2013;38(5):757-761
OBJECTIVETo establish a method of TLC identification for Dida commonly used in Tibetan medicine from different species.
METHODWith silica gel G as the stationary phase, and chloroform-methanol (40: 1) as mobile phase, oleanolic acid from different species of Dida was separated and identified.
RESULTOleanolic acid was detected in 70 kinds of Dida derived from the Gentianaceae Swertia, Halenia, Gentianopsis, Lomatogonium, and Saxifragaceae saxifrage, except for the saxifrage, there are some differences among different genera or subjection.
CONCLUSIONThis TLC method can be used for identification of oleanolic acid in Dida from different species except saxifrage.
Chromatography, High Pressure Liquid ; Chromatography, Thin Layer ; methods ; Drugs, Chinese Herbal ; chemistry ; Medicine, Tibetan Traditional ; methods ; Oleanolic Acid ; analysis ; chemistry ; Species Specificity
7.Influence of storage period and grading standards on quality of Prunella vulgaris.
Yuhang CHEN ; Qiaosheng GUO ; Li LIU ; Chengya WANG
China Journal of Chinese Materia Medica 2012;37(7):882-886
OBJECTIVETo investigate the influence of storage period and grading standards on the quality of Prunella vulgaris in order to provide a theoretical basis for standardized cultivation.
METHODThe spices of P. vulgaris in different storage period (including current year, first-year and second-year) were collected from Lujiang base in Anhui Province. The samples were randomized, with the methods of morphologic characteristics and commercial size on P. vulgaris, the samples were graded into three grades; according to the methods from the Pharmacopoeia of the People's Republic of China, water-soluble extracts, ethanol-soluble extracts, total ash and acid insoluble ash were measured, respectively, utilizing the UV spectrophotometry to detection the contents of total flavonoids and polysaccharides, the levels of ursolic acid, oleanolic acid and rosmarinic acid were adopted by HPLC.
RESULTThe total ash and acid insoluble ash of P. vulgaris showed significantly increase during prolonged storage; however, the content of water-soluble extracts, ethanol-soluble, total flavonoids, polysaccharides, ursolic acid, oleanolic acid,rosmarinic acid showed significantly decrease during prolonged storage. The spica of P. vulgaris exhibited no rules differences between the quality and grading standards, The second-degree belongs to high content of total flavonoids; the high content of polysaccharides was first-degree; the total ash and acid insoluble ash of spicas exhibited gradually decreased from first-degree to third-grade, and the content of water-soluble extracts, ethanol-soluble extracts,ursolic acid,oleanolic acid, rosmarinic acid showed gradually increased from first-degree to third-grade.
CONCLUSIONThe current year was a suitable storage time of spicas from P. vulgaris could be selected; and the main bioactive components highest level of P. vulgaris spicas was third-degree, second-grade next, first-degree minimum.
China ; Chromatography, High Pressure Liquid ; Cinnamates ; analysis ; Depsides ; analysis ; Drug Storage ; Flavonoids ; analysis ; Oleanolic Acid ; analysis ; Polysaccharides ; analysis ; Prunella ; chemistry ; Triterpenes ; analysis
8.Chemical constituents from Sambucus chinensis.
China Journal of Chinese Materia Medica 2012;37(10):1399-1401
Five compounds were separated from Sambucus chinensis and identified as maslinic acid(1), 12alpha, 13-dihydroxyolean-3-oxo-28-oic acid(2), 13-hydroxyolean-3-oxo-28-oic acid (3), 3-oxo oleanolic acid (4), corosolic acid (5). Of them,compound 3 was a new compound, and compounds 1, 2, 4, and 5 were seperated from this plant for the first time.
Oleanolic Acid
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analysis
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Sambucus
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chemistry
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Triterpenes
;
analysis
9.Chemical constituents of Halenia elliptica.
Hongling WANG ; Hao CHEN ; Chang'an GENG ; Xuemei ZHANG ; Yunbao MA ; Zhiyong JIANG ; Jijun CHEN
China Journal of Chinese Materia Medica 2011;36(11):1454-1457
OBJECTIVETo study the chemical constituents of Halenia elliptica.
METHODThe air-dried whole plants of Halenia elliptica were extracted with 90% EtOH. The EtOH extract was condensed to a small amount of volume and extracted with petroleum ether, EtOAc and n-BuOH, successively. The compounds were isolated and purified by column chromatography from the EtOAc fraction, and identified based on spectral analyses (MS, 1H-NMR, 13C-NMR).
RESULT12 compounds were isolated from H. elliptica, and characterized as 8-hydroxy-2-methylchromone (1), 5-methoxy-2-methylchromone (2), 7-epi-vogeloside (3), coniferl aldehyde (4), sinapaldehyde (5), norbellidifolin (6), 1-hydroxyl-2,3,4,6-tetramethoxyxanthone (7), 1-hydroxyl-2,3,4,7-tetramethoxyxanthone (8), 1-hydroxyl-2,3,5-trimethoxyxanthone (9), together with azelaic acid, beta-sitosterol, and oleanolic acid.
CONCLUSIONCompounds 1, 2 were new natural compounds and compounds 3-6, 10 were obtained from H. elliptica for the first time and compound 6 showed inhibitory activities against HBsAg and HBeAg secretion with IC50 value of 0.77 and < 0.62 mmol x L(-1), respectively.
Acrolein ; analogs & derivatives ; analysis ; isolation & purification ; Chromatography ; Dicarboxylic Acids ; analysis ; isolation & purification ; Gentianaceae ; chemistry ; Iridoid Glycosides ; isolation & purification ; Magnetic Resonance Spectroscopy ; Mass Spectrometry ; Oleanolic Acid ; analysis ; isolation & purification ; Plant Extracts ; isolation & purification ; Sitosterols ; analysis ; isolation & purification ; Xanthones ; analysis ; isolation & purification
10.Quality inspection of commercial Bupluri Radix samples in Guangzhou: an ELISA for determining saikosaponin A content using anti-saikosaponin A monoclonal antibody.
Li-ling MA ; Ming-ming TAN ; Zhi CHAO
Journal of Southern Medical University 2011;31(6):1006-1008
OBJECTIVETo inspect the quality of commercially available Chaihu (Bupluri Radix, a common traditional Chinese herbal drug) in Guangzhou by determining the content of saikosaponin A (SSa) using enzyme-linked immunosorbent assay (ELISA).
METHODSA competitive ELISA system using mouse anti-saikosaponin A monoclonal antibody was established for determining SSa content. Commercial samples of Chaihu were obtained from 10 drug stores in Guangzhou, and SSa contents in the methanol extracts of these samples were determined using the ELISA system.
RESULTSThe detection range of this competitive assay was 0.16-2.5 µg/ml for determining SSa contents. In the 10 commercial Chaihu samples, SSa contents in the methanol extract determined by this method ranged from 0.32 µg/mg to 6.87 µg/mg, and 3 samples showed a SSa content lower than the minimum requirement documented in the Chinese Pharmacopeia.
CONCLUSIONThis competitive ELISA is sensitive, rapid, economic and environment-friendly for SSa determination, especially suitable for batch determination. The results of SSa detection for the commercial Chaihu samples demonstrate an uneven quality of Chaihu in Guangzhou market, suggesting the necessity of more rigorous quality control measures for this drug.
Antibodies, Monoclonal ; Bupleurum ; chemistry ; Drugs, Chinese Herbal ; analysis ; Enzyme-Linked Immunosorbent Assay ; methods ; Oleanolic Acid ; analogs & derivatives ; analysis ; Quality Control ; Saponins ; analysis

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