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OBJECTIVE To establish the method for the content determination of 5-hydroxymethylfurfural （5-HMF） in glucosamine hydrochloride tablets， and to analyze its regularity and influential factors. METHODS Quantitative analysis of 5-HMF was performed using high-performance liquid chromatography. The analysis was conducted on Shim-pack GIST C18-AQ column with mobile phase consisted of 0.1% phosphoric acid solution-methanol （90∶10， V/V） at the flow rate of 1.0 mL/min. The column temperature was 30 ℃， and detection wavelength was 284 nm. The injection volume was 20 μL. Reaction kinetics test of different temperatures was adopted to analyze the relationship of 5-HMF content with reaction temperature and reaction time， and utilized to build its formation kinetic model. RESULTS The linger range of 5-HMF was 0.057-5.698 μg/mL （r＝0.999 9）. The limits of detection and quantitation were 5.70 and 17.09 ng/mL； RSDs of precision， repeatability and stability （24 h） tests were all lower than 1.0% （n＝6）. The average recoveries ranged from 99.38% to 99.73%（RSD＝0.53%， n＝9）. The contents of the 5-HMF in 8 batches of samples ranged 4.10-35.13 μg/g. Results of data fitting in reaction kinetics test showed that the higher reaction temperature and the longer reaction time， the higher 5-HMF content in the sample. At 50， 60， 70 and 80 ℃ ， the relationship between the content of 5-HMF and the reaction time was linear， in accordance with a zero-order kinetic model. The reaction rate constants were 6.789， 7.715， 8.815 and 11.430， respectively. CONCLUSIONS The established method has strong specificity， high sensitivity， and good accuracy； the reaction temperature and reaction time are important influential factors for the formation of 5-HMF in glucosamine hydrochloride tables. The change rule of its content conforms to the zero-order kinetic model.
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Objective: To establish chemical fingerprint and multi-components determination of 15 batches of Taohong Siwu Decoction (TSD), and provide reference for the improvement of its quality control. Methods: The separation was performed on Thermo Hypersil Gold C18 column (250 mm × 4.6 mm, 5 μm) for gradient elution with methanol-0.1% phosphoric acid aqueous solution, flow rate 1.0 mL/min, column temperature 30 ℃, and detection wavelength 225 nm. The HPLC fingerprint was established and evaluated by the similarity evaluation system of TCM (version 2012A), and the difference of chemical information between 15 batches of different samples was evaluated by cluster analysis. Furthermore, the content of the nine active components in the sample was determined by HPLC multi-component wavelength switching method, with the partial least squares-discriminant analysis (PLS- DA) by SIMCA 14.1 software to find significant components of the quality between the batches. Results: The HPLC fingerprint of 15 batches of TSD was established. The similarity was greater than 0.96, and 35 common peaks were identified as gallic acid, chlorogenic acid, amygdalin, albiflorin, hydroxysafflor yellow A, paeoniflorin, ferulic acid, senkyunolide I, benzoylpaeoniflorin and ligustilide (corresponding to peaks 2, 8, 9, 13, 14, 15, 16, 25, 31, and 32). The linearity relationships of gallic acid, 5-hydroxymethylfurfural, chlorogenic acid, albiflorin, hydroxysafflor yellow A, paeoniflorin, ferulic acid, verbascoside, and senkyunolide I (r ≥ 0.999 6) were good. The results of content determination respectively were 187.5-344.4, 6.2-154.8, 413.2-459.2, 507.5-923.5, 873.8-1 202.0, 2 122.3-2 782.9, 59.2-121.3, 6.4-26.9, and 38.9-79.6 μg/g, respectively, including higher content of paeoniflorin, hydroxysafflor yellow A, and albiflorin. Furthermore, 15 batches of samples from different origins were classified into three categories. Using PLS-DA analysis, the content determination result showed that paeoniflorin, albiflorin, hydroxysafflor yellow A, and 5-hydroxymethylfurfural were the four components that affected the quality of different batches of TSD. Conclusion: HPLC fingerprint combined with multi-components determination is suitable for quality control and evaluation of TSD preparation.
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Objective: To establish an HPLC fingerprint of Qingxin Zishen Prescription Decoction (QZPD) and determine the contents of its multiple components, so as to provide a scientific basis for quality control. Methods: HPLC analysis was performed on a Phenomenex Kinetex C18 column (100 mm × 4.60 mm, 2.6 μm) for gradient elution with the mobile phase consisting of methanol, acetonitrile and 0.2% formic acid aqueous. The detection wavelength was set at 245 nm and 280 nm, and the column temperature was 40 ℃. Fingerprints of ten batches of QZPD were determined, and the similarities among fingerprints were evaluated. Attributive analysis and identification of common peaks were performed and the contents of 15 components were determined. Results: The fingerprint similarities of 10 batches of QZPD were ranged from 0.923 to 0.998 compared with the reference fingerprint, and 33 common peaks were identified in the fingerprint. Among them, seven peaks (P11, P14-P16, P24, P29, P30) were identified from Coptidis Rhizoma, two peaks (P7, P19) were identified from Nelumbinis Plumula, two peaks (P14, P21) were identified from Ziziphi Spinosae Semen, nine peaks (P4, P5, P10, P17, P18, P28, P31-P33) were identified from Salvia miltiorrhiza, nine peaks (P1-P3, P6, P8, P9, P12, P13, P20) were identified from Corni Fructus, while five peaks (P22, P23, P25-P27) cannot be originated and none of the common peaks was identified from Rehmanniae Radix, Uncariae Ramulus Cum Uncis and Triticum aestivum. By comparing with the chemical reference, fifteen components, including gallic acid (P2), 5-hydroxymethylfurfural (P3), danshensu (P4), protocatechuic aldehyde (P5), morroniside (P9), caffeic acid (P10), cornin (P12), loganin (P13), magnoflorine (P14), coptisine (P24), lithospermic acid (P28), berberine (P29), palmatine (P30), salvianolic acid B (P31) and salvianolic acid E (P33), were identified and quantified. The contents of the fifteen components were 158.3-248.2, 233.6-321.3, 45.9-166.0, 24.3-38.6, 800.7-1 263.6, 26.6-54.9, 44.5-108.2, 470.4-757.3, 85.6-178.6, 11.1-34.2, 56.2-106.4, 25.9-138.9, 21.0-59.2, 951.6-2 244.7 and 38.6-92.8 μg/g, respectively. Conclusion: The method established in this study is stable and highly reproducible, and can provide basis for quality control of QZPD.
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Objective: To establish HPLC fingerprint of Eriobotryae Folium standard decoction and compare quality difference between raw and honey processed Eriobotryae Folium standard decoction, which can provide a reference for its quality control. Methods: An HPLC-DAD method was utilized. The mobile phase was acetonitrile-0.4% phosphoric acid setting for gradient elution. The HPLC fingerprints of 20 batches of standard decoction of raw and honey processed Eriobotryae Folium were established. The contents of neochlorogenic acid, chlorogenic acid, and cryptochlorogenic acid were determined simultaneously. Similarity and cluster analysis were chosen to evaluate the quality of standard decoction of raw and honey processed Eriobotryae Folium. Results: Both of the fingerprint and the contents of three kinds of chlorogenic acids of Eriobotryae Folium standard decoction had significant difference before and after the Eriobotryae Folium being processed by honey. Two chromatographic peaks were increased newly in honey processed Eriobotryae Folium. The No.1 peak refers to component of 5-hydroxymethylfurfural. The average contents of neochlorogenic acid, chlorogenic acid and cryptochlorogenic acid in raw Eriobotryae Folium standard decoction were 4.300, 4.306, and 5.432 mg/g respectively. The result of contents showed a significantly decrease in honey processed Eriobotryae Folium standard decoction. Their contents were 3.295, 3.460, and 4.118 mg/g respectively. The reduction rate of them were 23.29%, 19.06%, and 23.92% respectively. Conclusion: The method is concise and durable. It could not only be utilized to evaluate the quality of standard decoction of Eriobotryae Folium before and after processed by honey, but also to identify the quality differences of them. The study could be used for quality control of standard decoction of raw and honey processed Eriobotryae Folium, identify the quality difference of them and also provide a reference for quality control of their preparations.
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Objective: To identify the influencing factors (light, temperature, etc) of Guanxinning Injection (GXNI) in the storage and transportation process, and lay the foundation for the storage and transportation of GXNI. Methods: Taking the content of sodium danshensu, protocatechuic aldehyde, ferulic acid, rosmarinic acid, and salvianolic acid B as quantitative indicators, combined with the common peak similarity analysis, principal component analysis, and relative content comparison in the fingerprint to evaluate the effect of different influencing factors on the main chemical composition of GXNI. Results: After low temperature treatment, the content of four compounds, such as senkyunolide I and senkyunolide H, were increased, the content of five compounds, such as vanillic acid and vanillin aldehyde, were reduced, the content of 13 compounds, such as protocatechuic aldehyde and ferulic acid, showed no significant changes. Under the freezing-thawing conditions, the content of four compounds, such as 5-hydroxymethylfurfural, were increased, the content of seven compounds, such as vanillin acid and chlorogenic acid, was reduced, the content of 11 compounds, such as sodium danshensu and ferulic acid, showed no significant changes. Under high temperature, the content of seven compounds, such as sodium danshensu and protocatechuic aldehyde, were increased, the content of 11 compounds, such as ferulic acid and rosmarinic acid, were reduced, the content of four compounds, such as chlorogenic acid and caffeic acid, showed no significant changes. Under strong light conditions, the content of two compounds, such as senkyunolide H, were increased, the content of 16 compounds, such as ferulic acid and salvianolic acid B, were reduced, the content of four compounds, such as sodium danshensu and protocatechuic aldehyde, showed no significant changes. Conclusion: High temperature and strong light will affect the components of GXNI, and some compounds will also be affected under freezing-thawing conditions. Thus, the GXNI should be stored under low temperature, but higher than 0 ℃.
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Objective:To establish the HPLC fingerprint of raw products,rice-processed products and honey-processed products of Codonopsis Radix from Shanxi,and establish determination of their chemical constituents,which was used to analyze the changes of types and contents of chemical constituents in Codonopsis Radix from Shanxi before and after processing. Method:Agilent ZORBAX SB-C18 column(4.6 mm×250 mm,5 μm) was adopted,the separation process was carried out using a binary gradient elution system composed of 0.5% phosphoric acid aqueous solution and acetonitrile,the column temperature was 30℃ and the detection wavelength was 220 nm. Result:Compared with the corresponding reference fingerprint,the similarities of HPLC fingerprint of 10 batches of raw products and processed products were >0.90.In raw products,rice-processed products and honey-processed products of Codonopsis Radix from Shanxi,the contents of lobetyolin were (0.33±0.049),(0.24±0.034),(0.18±0.047) mg·g-1,the contents of atractylenolide Ⅲ were (0.20±0.046),(0.40±0.046),(0.31±0.060) mg·g-1,the contents of 5-hydroxymethylfurfural(5-HMF) were (0.74±0.16),(1.45±0.19),(1.54±0.12) mg·g-1,respectively. Conclusion:Different processing methods have little effect on types of chemical constituents in Codonopsis Radix from Shanxi,but have great effect on the contents of some chemical constituents.
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Objective:To explore the correlation between colors and contents of water and 5-hydroxymethylfurfural (5-HMF) in Ginseng Radix et Rhizoma Rubra (GRRR). Method:The colors were observed under sunlight on a sheet of white paper. The chroma value and color difference were determined and calculated by a colorimeter. Water content was determined by the oven-drying method. An HPLC method was established and used to determine the content of 5-HMF. The correlation was analyzed by the Spearman and Pearson analysis. Result:The colors of GRRR were yellowish-white,ocher-yellow,and yellowish-brown. The values of L*,a*,b*,and ΔE* had a certain range, and could reflect the colors of GRRR. The content of water ranged from 4.01%to 8.31%and was in accordance with the requirement the Chinese Pharmacopoeia. The content of 5-HMF ranged from below the limit of detection (1.985×10-4 μg) to 78.97 μg·g-1. The results of correlation analysis shows significant correlations between L*,a*,b*, ΔE* values and water content, that is to say,the deeper the color was, the higher the content of water was,but with no significant correlation with 5-HMF content. Conclusion:The color of processed GRRR was related to water content but not related to 5-HMF content,which was not consistent with the correlation between color and 5-HMF content that generally existed in a series of raw Chinese medicinal materials. It indicated an essential difference between the color shade of processed Chinese medicinal materials and the cause of color change of raw Chinese medicinal materials. Therefore,it was significant to control water content for ensuring the stability of GRRR. This study determined the colors of GRRR by a colorimeter, systematically determined 5-HMF content,and proposed the effect of water contents on the color of GRRR.
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Some samples of Asparagi Radix were collected from medical markets.Colors of Asparagi Radix were observed by human vision and recorded to judge whether samples were degenerative.Water content of Asparagi Radix was determined by a drying method.The chroma value and color difference were determined and calculated by a colorimeter.With the deepening of color,the L*value was decreased and a*and ΔE*values were increased.It showed that the results determined by colorimeter can replace the results of visual observation.An HPLC method was established and used to determine the contents of 5-hydroxymethylfurfural(5-HMF) in Asparagi Radix.The results showed the 5-HMF contents were from 0.002 255 to 0.049 14 mg·g-1 in some samples with yellowish-white or yellowish-brown color,significantly increased from 0.080 80 to 0.105 1 mg·g-1 in some samples with brown color,and up to 1.033 mg·g-1 in an oil-spilling sample with dark brown color.This result demonstrated that the 5-HMF contents were significantly increased by accompanied with the deepening of color.There were the significant negatively correlation between the 5-HMF content and the L*value(P<0.01) and positively correlation between the 5-HMF content and the a*or ΔE*value(P<0.01) by the spearman analysis.The oil-spilling and qualified samples were clustered into two alone categories by the cluster analysis.That the limited standards of the 5-HMF content is not higher than 0.02% by HPLC method and of the L*value is not less than 50 by colorimeter method were suggested for Asparagi Radix.It is firstly reported the multiple-factor analysis about oil-spilling and discoloration and the establishment of limited standard of Asparagi Radix.
Subject(s)
Asparagus Plant , Chemistry , Chromatography, High Pressure Liquid , Color , Drugs, Chinese Herbal , Reference Standards , Plant Roots , ChemistryABSTRACT
Objective: To investigate the Maillard reaction products and anti-oxidant activity of dichloromethane extraction from Polygonati Rhizoma (PR) after processing. Methods: Three species of PR were prepared by different processing time according to the preparation process of Pharmacopoeia of the People's Republic of China. The colour changes of Maillard reaction characteristics during the processing of PR were detected by UV-Vis; The pH changes were detected by pH detector; GC-MS was used to analyze the change of Maillard reaction products (MRPs); DPPH radical scavenging activity was used as the evaluation index of anti-oxidant activity. Results: With the increase of processing time, the MRPs and Browning degree increased, the pH value decreased, and the anti-oxidant activity increased. After processing for 16 h, three species of PR had the same change, showing the characteristics of Maillard reaction. GC-MS analysis detected multiple characteristic MRPs, including 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran- 4-one and 5-hydroxymethylfurfural. The DPPH radical scavenging activities of three species of PR were significantly increased after processing for 16 h. Conclusion: During the processing, PR have the characteristic products in Maillard reaction, and with the extension of processing time, the anti-oxidant activity increases regularly. These provide a basis for the material basic research of PR.
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Objective: To establish an HPLC method for the analysis of thirteen main chemical constituents (gallicacid, 5-hydroxymethylfurfural, methylgallate, oxypaeoniflora, catechins, paeoniflorin, 1,2,3,6-tetra- O-galloyl-D-glucose, 1,2,4,6-tetra-O- galloyl-D-glucose, benzoicacid, 1,2,3,4,6-penta-O-galloyl-D-glucose, mudanpioside C, benzoyloxypaeoniflorin, and paeonal) in Moutan Cortex from different origins. Methods: The methanol (50%) reflux extraction was adopted to Moutan Cortex. Separation was carried out on C18 (250 mm × 4.6 mm, 5 μm), the mobile phase was eluted with acetonitrile-0.5% phosphoric acid. The flow rate was 1.0 mL/min, the detection wavelength was 254 nm, and the column temperature was 30 ℃. Results :The linear relation of thirteen main active components measured in the range of mass concentration was good with perfect precision, repeatability, and stability, the value of which was all more than 0.999 5. Conclusion: The HPLC method established for simultaneous determination of thirteen main chemical compositions in Mortan Cortex is effective, accurate, and reproducible, which can be used for the quality control of Mortan Cortex.
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Objective: To explore the therapeutic effects of different extracts of Eucommia ulmoides on Parkinson’s disease mice, as well as the relationship between ultra-high performance liquid chromatography (UPLC) fingerprint and treatment of Parkinson’s disease. Methods Through the mouse climbing test and the content of dopamine (DA) in the striatum of the brain, the therapeutic effect of different gradient ethanol extracts of E. ulmoides on Parkinson’s disease mice was observed. Ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) was used to analyze the fingerprints of different extracts of E. ulmoides. Combined with the results of climbing rod test and dopamine content, partial least squares regression (PLSR) analysis was used to establish the pharmacodynamic relationship between E. ulmoides and Parkinson’s disease. Results The 50% and 75% ethanol extracts of E. ulmoides could significantly shorten the climbing time. The 75% ethanol extract of E. ulmoides significantly increased the striatum dopamine content in the brain. The results of PLSR analysis showed that ulmoside, liriodendrin, 5-hydroxymethylfurfural, caffeic acid in E. ulmoides were closely related to climbing rod and dopamine content of mice. Conclusion The ethanol extract of E. ulmoides has anti-Parkinson’s disease effect, and the effect is most significant with 75% alcohol extract. The compounds of ulmoside, liriodendrin, 5-hydroxymethylfurfural, caffeic acid may be the main active ingredients of E. ulmoides in the treatment of Parkinson’s disease.
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Objective To establish a combinative method based on HPLC fingerprint, multi-component assay, and pattern recognition for quality evaluation of Sparganii Rhizoma. Methods The similarity analyzed with “Similarity Evaluation System for Chromatographic Fingerprint of Chinese Materia Medica 2004A”, Nine kinds of components were identified by comparison with reference substances and their content in samples were determined and hierarchical clustering analysis (HCA) and principal component analysis (PCA) were performed by SPSS 20.0. Results There were 12 common peaks, and the similarity degrees of 12 batches of samples were more than 0.800, which showed that all the samples from different origins were of good consistency. Nine of them were identified as 5-hydroxymethylfurfural, vanillic acid, ferulic acid, p-hydroxybenzaldehyde, p-hydroxybenzoic acid, vanillin, protocatechuic acid, p-coumaric acid, and isoferulic acid; The samples were divided into four clusters by HCA. The result of PCA showed, the quality of samples could be evaluated basically. According to the composite score, the quality of Sparganii Rhizoma from different origins, Henan Xinxiang, Jiangsu Zhenjiang, Hebei Cangzhou, Hunan Yueyang, Zhejiang Jinhua, and Henan Zhengzhou were better than others. There was a correlation between the scores of the main components of the 12 batches of decoction pieces and the results of the content determination. Conclusion The method is simple, reproducible, and reliable, it can be used for quality control and evaluation of Sparganii Rhizoma from different origins.
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Objective: A method for simultaneous determination of 10 active ingredients in Dahuang Lidan Tablets (DLP) by HPLC wavelength switching method was established, and its quality was evaluated by statistical analysis. Methods: A Phenomenex Kinetex C18 column was used with a column temperature of 30 ℃ and a mobile phase gradient of methanol-0.15% phosphoric acid. The flow rate was 1 mL/min and the detection wavelengths were 265.0 nm (0-5.8 min, gallic acid), 283.9 nm (5.8-7 min, 5-hydroxymethyl furfural), 222.2 nm (7-18 min, corilagin, p-hydroxybenzaldehyde), 256.7 nm (18-74 min, ellagic acid, aloe-emodin, rhein, emodin, chrysophanol, emodin methyl ether), respectively. Statistical analysis of the content of components in 10 batches of drugs was performed using SPSS 21 Software. Results: The linearity of 10 components in the respective mass concentration ranges was good (r > 0.998 0), the average sample recovery was in the range of 98.45%-100.12%, and the RSD was in the range of 0.80%-2.51%. The content of 10 components was as follow: gallic acid (8.371-11.438 mg/tablet), 5-hydroxymethylfurfural (0.046-0.087 mg/tablet), corilagin (0.721-2.094 mg/tablet), p-hydroxybenzaldehyde (0.034-0.065 mg/tablet), ellagic acid (1.736-1.996 mg/tablet), aloe-emodin (0.337-0.440 mg/tablet), rhein (1.636-2.562 mg/tablet), emodin (0.602-0.846 mg/tablet), chrysophanol (0.388-0.566 mg/tablet) and emodin methyl ether (0.621-0.781 mg/tablet). The quality of the 10 batches of samples was basically the same. Conclusion: This method is simple and accurate and can be used for the quality control of DLP.
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Objective: To optimize the water extraction process of Siwu Decoction by BP neural network combined with orthogonal experiment. Methods: The water amount, the extraction time, and the extraction times were taken as factors. Entropy weight method was used to calculate the comprehensive scores of the multi-indicators of eight active components of 5-hydroxymethylfurfural, chlorogenic acid, caffeic acid, paeoniflorin, ferulic acid, verbascoside, senkyunolide A, and ligustilide in R language environment. Using comprehensive score as an evaluation indicator, the BP neural network model was established by orthogonal experiment design, and the optimal water extraction process of Siwu Decoction was predicted through network training. Results: The optimized extraction process of Siwu Decoction was carried out by adding 8 times of water and extracting 3 times for 1 h. The relative error between the network predicted value and the actual measured value of the test sample was less than 1%. Conclusion: The established mathematical model can analyze and predict the water extraction process of Siwu Decoction. The obtained process is stable and feasible, and can effectively extract the active ingredients in Siwu Decoction.
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Objective: To establish the fingerprint chromatography of Shujin Huoxue products (Shujin Huoxue Capsule and Shujin Huoxue Tablet) and provide a reference for its overall quality evaluation. Methods: The analysis was performed on Agilent Poroshell 120 SB-C18 (150 mm × 4.6 mm, 2.7 μm) column with acetonitrile-0.2% formic acid solution for gradient elution, the flow rate was 0.5 mL/min, the detection wavelength was 277 nm, and the column temperature was 30 oC. HPLC of 23 batches of Shujin Huoxue products were analyzed by the software “Similarity Evaluation System for Chromatographic Fingerprint of TCM (2012 edition)” combined with principal component analysis (PCA), cluster analysis (CA), and orthogonal partial least squares discriminant analysis (OPLS-DA). Results: The similarity of 18 batches (S1-S17 and S23) of samples was more than 0.900, 23 batches of samples could be clustered into three groups by PCA, CA, and OPLS-DA analysis. Among these, S1-S16 were clustered into group I, S23 and S17 could be divided into group II, and S18-S22 were clustered into group III. Four common peaks with larger differences were determined from 10 common peaks, including peaks 1, 3 (5-hydroxymethylfurfural), 6 (phenylacetic acid), and 10 (4-methoxy salicylaldehyde). Conclusion: Fingerprint chromatography combined with chemical pattern recognition technique was stable and simple, which could be used to evaluate the quality of Shujin Huoxue products systematically and comprehensively.
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OBJECTIVE： To establish a method for simultaneous determination of eleven active constituents in Zhenwutang decoction， such as 5-hydroxymethylfurfural， （+）-cianidanol， paeoniflorin， benzoylaconitine， benzoylhypacoitine， benzoylpaeoniflorin， 6-gingerol， 8-gingerol， atractylenolide Ⅱ， 6-shogaol and pachymic acid. METHODS： HPLC method was adopted. The separation was performed on Phenomenex Kinetex C18 column with mobile phase consisted of acetonitrile-0.2 ％ phosphoric acid solution（gradient elution） at flow rate of 1.0 mL/min. The detection wavelength was set at 285 nm （4.4-7 min， 5-hydroxymethylfurfural）， 203 nm [7-12 min，（+）-cianidanol]， 233 nm （12-50 min，paeoniflorin， benzoylaconitine， benzoylhypacoitine， benzoylpaeoni- florin）， 200 nm （50-62.3 min， 6-gingerol， 8-gingerol； 62.9-90 min， 6-shogaol， pachymic acid） and 222 nm （62.3-62.9 min， atractylenolide Ⅱ）. The column temperature was set at 35 ℃， and the sample size was 20 μL. RESULTS： The linear ranges of 5-hydroxymethylfurfural， （+） -cianidanol， paeoniflorin， benzoylaconitine， benzoylhypacoitine， benzoylpaeoniflorin， 6-gingerol， 8-gingerol， atractylenolide Ⅱ， 6-shogaol， pachymic acid were 0.62-12.47 μg/mL （r＝0.999 6），2.36-47.25 μg/mL （r＝0.999 7），200.80-4 016 μg/mL （r＝0.999 7），4.45-89.04 μg/mL （r＝0.999 6），4.28-85.54 μg/mL （r＝0.999 5），5.16-103.13 μg/mL （r＝0.999 9），5.53-110.66 μg/mL （r＝0.999 9），0.84-16.89 μg/mL （r＝0.999 8），0.60-12.04 μg/mL （r＝0.999 9），0.53-10.62 μg/mL （r＝0.999 5），1.04-20.78 μg/mL （r＝0.999 7）， respectively. The limits of quantitation were 0.155， 0.590， 1.210， 1.112， 1.070， 0.258， 0.553， 0.421， 0.153， 0.354， 0.431 μg/mL， respectively. The limits of detection were 0.047， 0.179， 0.134， 0.337， 0.324， 0.078， 0.168， 0.128， 0.046， 0.107， 0.131 μg/mL， respectively. RSDs of precision， stability and reproducibility tests were all lower than 3％. The average recovery rates were 96.06％-103.01％（RSD＝2.64％，n＝6）， 95.11％-101.57％（RSD＝2.58％，n＝6）， 97.22％-102.11％（RSD＝1.93％，n＝6）， 96.43％-102.78％（RSD＝2.35％，n＝6）， 96.42％-101.43％（RSD＝2.15％，n＝6）， 96.86％-102.05％（RSD＝2.10％，n＝6）， 95.32％-100.55％（RSD＝1.87％，n＝6）， 97.04％-103.25％（RSD＝2.22％，n＝6）， 96.78％-103.22％（RSD＝2.62％，n＝6）， 97.04％-103.14％（RSD＝2.28％，n＝6）， 97.08％-103.51％（RSD＝2.94％，n＝6）， respectively. CONCLUSIONS： The method is accurate and specific， and suitable for simultaneous determination 11 active components of Zhenwutang decoction.
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Objective: To investigate the causes and influencing factors of 5-hydroxymethylfurfural (5-HMF) during the processing of Cervi Cornu Pantotrichum (CCP). Methods: HPLC was used to determine the content of 5-HMF in CCP with different processing methods and different parts. Moreover, the contents of total sugar, reducing sugar, amino acid, and Ca, Mg, Fe, and Cu in velvet antler were determined, and the effects of several factors on 5-HMF production during processing were discussed by comparing the contents of above mentioned substances in velvet antler with different processing methods. Results: The contents of 5-HMF of boiled CCP were significantly higher than that of freeze-dried CCP (P < 0.05) in same parts, indicating that high temperature intensified caramelization reaction and Maillard reaction to produce more 5-HMF in boiled CCP; The contents of 5-HMF of CCP with blood were significantly higher than that of CCP without blood (P < 0.05), CCP with blood was rich in total sugar, reducing sugar and amino acid and these substances can provide sufficient substrate to produce more 5-HMF; The content of 5-HMF in wax slices was significantly higher than other parts (P < 0.05), and rich content of total sugars, reducing sugars, amino acids, and differentially distributed mineral elements all contribute to the production of 5-HMF in wax slices. Conclusion: The production of 5-HMF in processing CCP is the result of the combined action of total sugar, reducing sugar, amino acid, and mineral elements at different temperatures.
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AIM To establish a quantitative analysis of multi-components by single mark (QAMS) method for the simultaneous content determination of five constituents in Shanzhuyu Formulated Granules (Corni Fructus).METHODS The analysis of 80％ methanol extract of this drug was performed on a 30 ℃ thermostatic Wondasil C18column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.3％ phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 335 nm.With morroniside as an internal standard,the relative correction factors of gallic acid,5-hydroxymethylfurfural,loganin and cornuside were established,followed by the determination of their contents.RESULTS Gallic acid,5-hydroxymethylfurfural,morroniside,loganin and cornuside showed good linear relationships within the ranges of 0.0120-0.120,0.026 8-0.268,0.074 4-0.744,0.058 6-0.586 and 0.0086-0.086 μg (r≥ 0.9999),whose average recoveries (RSDs) were 103.43％ (1.45％),103.36％ (1.50％),104.47％ (0.30％),102.08％(1.74％) and 104.01％ (0.62％),respectively.The results obtained by QAMS approximated those obtained by external standard method.CONCLUSION This stable and reliable method can be used for the quality control of Shanzhuyu Formulated Granules.
ABSTRACT
AIM To establish a quantitative analysis of multi-components by single mark (QAMS) method for the simultaneous content determination of five constituents in Shanzhuyu Formulated Granules (Corni Fructus).METHODS The analysis of 80％ methanol extract of this drug was performed on a 30 ℃ thermostatic Wondasil C18column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.3％ phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 335 nm.With morroniside as an internal standard,the relative correction factors of gallic acid,5-hydroxymethylfurfural,loganin and cornuside were established,followed by the determination of their contents.RESULTS Gallic acid,5-hydroxymethylfurfural,morroniside,loganin and cornuside showed good linear relationships within the ranges of 0.0120-0.120,0.026 8-0.268,0.074 4-0.744,0.058 6-0.586 and 0.0086-0.086 μg (r≥ 0.9999),whose average recoveries (RSDs) were 103.43％ (1.45％),103.36％ (1.50％),104.47％ (0.30％),102.08％(1.74％) and 104.01％ (0.62％),respectively.The results obtained by QAMS approximated those obtained by external standard method.CONCLUSION This stable and reliable method can be used for the quality control of Shanzhuyu Formulated Granules.
ABSTRACT
AIM To study the effects of Rehmanniae Radix Preparata (A) and Poria (B) on decoction amounts of loganin,morroniside and 5-hydroxymethylfurfural in Corni Fructus (C).METHODS These three medicinal materials were combined one another and divided into seven groups (A,B,C,A + B,A + C,B + C and A + B + C).Then the contents of three constituents were determined by HPLC.RESULTS Compared with the single decoction of Corni Fructus,the decoction amounts of loganin and 5-hydroxymethylfurfural were decreased,and that of morroniside was increased at the time of mixed decoction of Rehmanniae Radix Preparata and Corni Fructus,or Rehmanniae Radix Preparata,Poria and Corni Fructus.This situation was just the contrary at the time of mixed decoction of Poria and Corni Fructus.CONCLUSION The mixed decoction of Corni Fructus,Rehmanniae Radix Preparata and Poria increases the decoction amount of morroniside,which may make mixed decoction liquid show better efficacy.