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1.
Article in Chinese | WPRIM | ID: wpr-943095

ABSTRACT

ObjectiveTo analyze changes of the chemical composition in Euodiae Fructus before and after processing with Coptidis Rhizoma decoction, so as to provide scientific basis for elucidating the processing mechanism of this decoction pieces. MethodUltra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS) was performed on a Titank C18 column (2.1 mm×100 mm, 1.8 μm), the mobile phase was 0.1% formic acid aqueous solution-acetonitrile for gradient elution, the column temperature was set at 40 ℃, the flow rate was 0.25 mL·min-1. Electrospray ionization (ESI) was used to scan in positive and negative ion modes, and the scanning range was m/z 50-1 250. The chemical constituents in Euodiae Fructus were identified before and after processing by reference substance comparison, database matching and literature reference, and MarkerView™ 1.2.1 software was used to normalize the obtained data, SIMCA-P 14.1 software was employed to perform principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) on MS data of raw and processed products to screen the differential components before and after processing. ResultA total of 50 compounds were identified, including 48 kinds of stir-fried products with Coptidis Rhizoma decoction and 44 kinds of raw products. After processing, six compounds were added, including danshensu, noroxyhydrastinine, oxyberberine, 13-methylberberrubine, protopine and canadine. However, two kinds of compounds, including (S)-7-hydroxysecorutaecarpine and wuchuyuamide Ⅱ, were not detected after processing. In general, after processing, the overall contents of phenolic acids and flavonoids decreased significantly, the overall content of limonoids increased, and the overall content of alkaloids did not decrease insignificantly. The results of PCA and OPLS-DA showed that there were significant differences in the composition and content of the chemical components of Euodiae Fructus before and after processing, and a total of 12 variables such as quercetin, dihydrorutaecarpine and dehydroevodiamine were obtained by screening. ConclusionEuodiae Fructus stir-fried with Coptidis Rhizoma decoction mainly contains phenolic acids, flavonoids, limonoids and alkaloids. The composition and content of the chemical components have some changes before and after processing. The addition of processing excipients and hot water immersion are the main reasons for the difference, which can provide experimental basis for interpretation of the processing mechanism of this characteristic processed products of Euodiae Fructus.

2.
Article in Chinese | WPRIM | ID: wpr-942336

ABSTRACT

ObjectiveTo analyze the flavor substances and change rules of Rhei Radix et Rhizoma during the process of nine-time repeating steaming and sun-drying. MethodThe flavor response values of Rhei Radix et Rhizoma samples were obtained by using PEN3 electronic nose system. The data were processed and analyzed by principal component analysis (PCA), linear discriminant analysis (LDA) and Loadings analysis. ResultRhei Radix et Rhizoma processed with nine-time repeating steaming and sun-drying could be effectively distinguished into two categories as the sixth sample was the turning point. The samples steamed and dried for one to five times could be grouped into one category, the other four samples were obviously distinguished from them. The main flavor components reached the maximum response in the sample processed with six-time repeating steaming and sun-drying, and its response value of inorganic sulfur compounds was about 2.7 times that of the sample processed with one-time repeating steaming and sun-drying. In addition, compared with the raw products, the flavors of Rhei Radix et Rhizoma processed with nine-time repeating steaming and sun-drying and wine stewing changed significantly, and the response value of inorganic sulfur compounds in sample processed with nine-time repeating steaming and sun-drying was about 2.2 times that of raw products. From the perspective of flavor analysis, the response values of inorganic sulfur compounds and nitrogen-oxygen compounds in sample processed with nine-time repeating steaming and sun-drying were higher than those of wine-stewed products, and the two were not completely equivalent. ConclusionElectronic nose technology preliminarily clarifies the dynamic change rules of the flavor of Rhei Radix et Rhizoma during the process of nine-time repeating steaming and sun-drying from the flavor characteristics, and clarifies the difference between products processed with nine-time repeating steaming and sun-drying and wine-stewed products from the odor characteristics, which lays a foundation for revealing the processing principle of Rhei Radix et Rhizoma processed with nine-time repeating steaming and sun-drying.

3.
Article in Chinese | WPRIM | ID: wpr-942334

ABSTRACT

ObjectiveTo compare the effects of different drying methods on volatile components of Pseudostellariae Radix. MethodThe samples were dried by different methods, including air drying, sun drying, hot air drying (40, 60, 80 ℃) and vacuum freeze drying. Gas chromatography-ion mobility spectrometry (GC-IMS) was used to compare the changes of volatile components in the samples after different treatments. The samples were incubated at 80 ℃ and 500 r·min-1 for 15 min, the injection temperature was 85 ℃, the injection volume was 200 μL, the flow rate of carrier gas was from 2 mL to 150 mL during 20 min, and the temperature of IMS detector was 60 ℃. SE-54 capillary column (0.32 mm×30 m, 0.25 μm) was used, the column temperature was 60 ℃, and the analysis time was 35 min. The differential spectra of volatile components were constructed and analyzed by principal component analysis (PCA). ResultA total of 37 volatile components were identified from dried Pseudostellariae Radix. The number of compounds in descending order was ketones, aldehydes and alcohols. There were some differences in the volatile components in samples dried by different methods. And the volatile components in samples with sun drying, air drying and hot air drying at 40 ℃ were similar, compared with other drying methods, vacuum freeze drying and hot air drying at 80 ℃ had great effects on the volatile components of Pseudostellariae Radix, and the compounds in the samples with vacuum freeze drying were the least. ConclusionIn this study, GC-IMS for the detection and analysis of volatile components in Pseudostellariae Radix is established, which has the characteristics of high efficiency, nondestructive inspection and simple sample processing. This method can be used for the distinction of Pseudostellariae Radix dried by different methods. And hot air drying at 40 ℃ can effectively retain the volatile components of Pseudostellariae Radix, and achieve similar flavor to samples with sun drying and air drying.

4.
Article in Chinese | WPRIM | ID: wpr-940527

ABSTRACT

ObjectiveA feedforward control model for dry granulation of polysaccharide components was established to guide the adjustment and optimization of critical process parameters (CPPs) in the design space, so as to reduce the impact of fluctuations in raw materials properties on the quality of medicines. MethodTaking Astragali Radix extract powder as the model drug, the design space of dry granulation CPPs was determined by Box-Behnken design. Astragali Radix mixed powder with different powder properties were prepared by mixture design, the variance inflation factor (VIF) was used to diagnose the multicollinearity of the powder properties, and principal component analysis (PCA) was used to extract the characteristic data of the model. Radial basis function neural network (RBFNN) was used to establish a feedforward control model for reflecting the relationship between the powder properties of polysaccharide components, dry granulation CPPs and one-time molding rate. ResultThe design space for dry granulation CPPs of polysaccharide components was 16-35 Hz for feeding speed, 10-23 Hz for roller speed, and 10-46 kg·cm-2 for roller pressure. The established RBFNN feedforward control model had a good predictive effect on the one-time molding rate of dry granulation of polysaccharide components, which could be used to guide the adjustment and optimization of CPPs in the design space, the relative error was 0.38%-6.73%, and the average relative error was 3.42%. ConclusionThe established feedforward control model can well reflect the relationship between the powder properties of the polysaccharide components, the dry granulation CPPs and the one-time molding rate of the granules, which can be used to guide the adjustment and optimization of CPPs in the design space, reduce the impact of material property fluctuation on product quality, and provide ideas for promoting the quality of traditional Chinese medicine from passive control to active control.

5.
Article in Chinese | WPRIM | ID: wpr-940216

ABSTRACT

ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water, the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea, and their processed products of rice-washed water. Chromatographic conditions were programmed temperature (starting temperature of 50 ℃ for 2 min, rising to 120 ℃ with the speed of 10 ℃·min-1, then rising to 170 ℃ at 2.5 ℃·min-1, and rising to 240 ℃ at 10 ℃·min-1 for 3 min), the inlet temperature was 280 ℃, the split ratio was 10∶1, and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization (EI) with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discriminant analysis (OPLS-DA) on each sample data, the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection (VIP) value>1. ResultA total of 60 components were identified, among which 40 were rhizomes of A. chinensis and 38 were its processed products, 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively, indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water, and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same, but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids, and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water, the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed, and pinene, 3-carene, p-cymene, ocimene, terpinolene, atractylon, acetic acid and furfural can be used as difference markers before and after processing.

6.
Article in Chinese | WPRIM | ID: wpr-940187

ABSTRACT

ObjectiveTo identify the chemical constituents of Alismatis Rhizoma before and after processing with salt-water by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS), and to investigate the changes of terpenoids in Alismatis Rhizoma before and after processing with salt-water. MethodUPLC-Q-TOF-MS was used to detect with 0.1% formic acid aqueous solution (A)-acetonitrile (B)as mobile phase for gradient elution (0-0.01 min, 20%B; 0.01-5 min, 20%-40%B; 5-40 min, 40%-95%B; 40-42 min, 95%B; 42-42.1 min, 95%-20%B; 42.1-45 min, 20%B), electrospray ionization (ESI) was selected for collection and detection in positive ion mode with the scanning range of m/z 100-1 250 and ion source temperature at 500 ℃. The data were analyzed by PeakView 1.2.0.3, the components were identified according to the primary and secondary MS data, and combined with the reference substance and literature. After normalized treatment by MarkerView 1.2.1, the MS data were analyzed by principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA), and then the differential components before and after processing were screened. The content changes of differential components were analyzed according to the relative peak area. ResultA total of 30 components were identified under positive ion mode, including 28 prototerpene triterpenes and 2 sesquiterpenes. The results of PCA and OPLS-DA showed that there were significant differences in components from Alismatis Rhizoma before and after processing with salt-water, and 10 differential components (alisol B 23-acetate, alisol I, alismol, 11-deoxy-alisol B 23-acetate, alisol B, alisol C, 11-deoxy-alisol B, alisol G, 11-deoxy-alisol C and alisol A) were screened, and the contents of alisol G and alisol A decreased significantly after processing. ConclusionUPLC-Q-TOF-MS can comprehensively and accurately identify the chemical constituents in raw and salt-processed products of Alismatis Rhizoma. It takes a great difference in the contents of chemical constituents before and after processing, and the difference of substituents is the main reason for this differences, which can provide reference for determining the material basis of efficacy changes of Alismatis Rhizoma before and after processing with salt-water.

7.
Article in Chinese | WPRIM | ID: wpr-940155

ABSTRACT

ObjectiveTo identify the chemical constituents of Alismatis Rhizoma before and after processing with salt-water by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS), and to investigate the changes of terpenoids in Alismatis Rhizoma before and after processing with salt-water. MethodUPLC-Q-TOF-MS was used to detect with 0.1% formic acid aqueous solution (A)-acetonitrile (B)as mobile phase for gradient elution (0-0.01 min, 20%B; 0.01-5 min, 20%-40%B; 5-40 min, 40%-95%B; 40-42 min, 95%B; 42-42.1 min, 95%-20%B; 42.1-45 min, 20%B), electrospray ionization (ESI) was selected for collection and detection in positive ion mode with the scanning range of m/z 100-1 250 and ion source temperature at 500 ℃. The data were analyzed by PeakView 1.2.0.3, the components were identified according to the primary and secondary MS data, and combined with the reference substance and literature. After normalized treatment by MarkerView 1.2.1, the MS data were analyzed by principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA), and then the differential components before and after processing were screened. The content changes of differential components were analyzed according to the relative peak area. ResultA total of 30 components were identified under positive ion mode, including 28 prototerpene triterpenes and 2 sesquiterpenes. The results of PCA and OPLS-DA showed that there were significant differences in components from Alismatis Rhizoma before and after processing with salt-water, and 10 differential components (alisol B 23-acetate, alisol I, alismol, 11-deoxy-alisol B 23-acetate, alisol B, alisol C, 11-deoxy-alisol B, alisol G, 11-deoxy-alisol C and alisol A) were screened, and the contents of alisol G and alisol A decreased significantly after processing. ConclusionUPLC-Q-TOF-MS can comprehensively and accurately identify the chemical constituents in raw and salt-processed products of Alismatis Rhizoma. It takes a great difference in the contents of chemical constituents before and after processing, and the difference of substituents is the main reason for this differences, which can provide reference for determining the material basis of efficacy changes of Alismatis Rhizoma before and after processing with salt-water.

8.
Article in Chinese | WPRIM | ID: wpr-940119

ABSTRACT

ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water, the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea, and their processed products of rice-washed water. Chromatographic conditions were programmed temperature (starting temperature of 50 ℃ for 2 min, rising to 120 ℃ with the speed of 10 ℃·min-1, then rising to 170 ℃ at 2.5 ℃·min-1, and rising to 240 ℃ at 10 ℃·min-1 for 3 min), the inlet temperature was 280 ℃, the split ratio was 10∶1, and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization (EI) with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discriminant analysis (OPLS-DA) on each sample data, the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection (VIP) value>1. ResultA total of 60 components were identified, among which 40 were rhizomes of A. chinensis and 38 were its processed products, 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively, indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water, and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same, but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids, and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water, the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed, and pinene, 3-carene, p-cymene, ocimene, terpinolene, atractylon, acetic acid and furfural can be used as difference markers before and after processing.

9.
Article in Chinese | WPRIM | ID: wpr-906060

ABSTRACT

Objective:Based on pharmacokinetics, the antitussive and expectorant related quality markers (Q-marker) of Trichosanthis Fructus were screened from diosmetin-7-<italic>O</italic>-glucopyranoside, diosmetin, apigenin, vanillic acid and cinnamic acid, and the candidate Q-marker was evaluated by multivariate statistical method. Method:Six healthy rats were randomly selected and the 70% ethanol extract of Trichosanthis Fructus (dose of 20 g·kg<sup>-1</sup>) was given by intragastric administration. Blood was collected from the orbital vein at different time points, and the plasma concentrations of 5 components (diosmetin-7-<italic>O</italic>-glucopyranoside, diosmetin, apigenin, vanillic acid and cinnamic acid) from Trichosanthis Fructus were detected simultaneously by high performance liquid chromatography-triple quadrupole tandem mass spectrometry (HPLC-QqQ-MS/MS). The main detection conditions were as following:mobile phase of 0.2% formic acid aqueous solution (A)-acetonitrile (B) for gradient elution (0-4 min, 6%-23%B; 4-5 min, 23%-59.5%B; 5-10 min, 59.5%-60%B), flow rate of 0.5 mL·min<sup>-1</sup>, the detection wavelength at 254 nm, electrospray ionization (ESI), positive ion mode detection, multiple reaction monitoring (MRM) mode scanning, scanning range of <italic>m</italic>/<italic>z</italic> 50-1 500. Diosmetin-7-<italic>O</italic>-glucopyranoside, diosmetin, apigenin and vanillic acid with clear pharmacokinetic behaviors were selected as candidate Q-marker about antitussive and expectorant of Trichosanthis Fructus. The contents of these components in 9 batches of medicinal materials were determined and the main detection conditions were the same as the pharmacokinetic study. SPSS 21.0 was used for cluster analysis and principal component analysis (PAC) based on the results of determination. Result:The pharmacokinetic results showed that the area under concentration-time curve (AUC<sub>0-</sub><italic><sub>t</sub></italic>) of 4 components (diosmetin-7-<italic>O</italic>-glucopyranoside, diosmetin, apigenin and vanillic acid) were (111.28±9.94), (27.08±2.76), (1 376.12±101.86), (631.32±64.72) μg·h·L<sup>-1</sup>, respectively. The 9 batches of Trichosanthis Fructus samples were clustered into 3 groups by systematic cluster analysis. The clustering results were related to the variety of Trichosanthis Fructus and also affected by the origin. The PCA results showed that the comprehensive scores of Gaotang Trichosanthis Fructus, Shanxi Trichosanthis Fructus, Hebei Ben Trichosanthis Fructus were 1.919, 1.356 and 0.299, respectively, ranking in the top 3 among all samples. The comprehensive scores of Nongkeyuan No. 1, Hebei Trichosanthis Fructus and Nongkeyuan No. 2 were -0.804, -1.085, -1.120, respectively, which were in the last 3 positions among all samples. Conclusion:The pharmacokinetic characteristics and quality evaluation of diosmetin-7-<italic>O</italic>-glucopyranoside, diosmetin, apigenin and vanillic acid meet the requirements about antitussive and expectorant related Q-marker of Trichosanthis Fructus.

10.
Article in Chinese | WPRIM | ID: wpr-905972

ABSTRACT

Objective:To establish the high performance liquid chromatography (HPLC) fingerprint of Citri Sarcodactylis Fructus, and to search for makers to characterize the quality difference of Citri Sarcodactylis Fructus from different origins coupled with chemometrics. Method:The analysis was performed on a Thermo Hypersil GOLD C<sub>18</sub> column (4.6 mm×250 mm, 5 μm) with mobile phase consisted of acetonitrile-0.05% phosphoric acid solution for gradient elution, and the detection wavelength was set at 254 nm. A total of 31 batches of samples were analyzed to establish the HPLC fingerprint of Citri Sarcodactylis Fructus. Similarity evaluation was performed by Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 edition) to confirm the common peaks, which were identified by comparison of reference substances. On the basis, chemometrics methods were used to analyze and evaluate the quality of Citri Sarcodactylis Fructus from different origins. At the same time, 3 batches of 5 species of decoction pieces from the genus <italic>Citrus</italic> in the family Rutaceae, including Citri Sarcodactylis Fructus, Aurantii Fructus Immaturus, Aurantii Fructus, Citri Reticulatae Pericarpium Viride and Citri Reticulatae Pericarpium, were randomly collected for evaluating the effectiveness and reliability of the established HPLC fingerprint of Citri Sarcodactylis Fructus. Result:HPLC fingerprint of Citri Sarcodactylis Fructus was established and 22 common peaks were identified. And seven common peaks among them were identified as 6,7-dimethoxycoumarin, diosmin, hesperidin, byakangelicin, 5,7-dimethoxycoumarin, bergapten and oxypeucedanin. Except for 2 batches of samples, the similarities of fingerprints between other 29 batches of samples were >0.9. The 31 batches of Citri Sarcodactylis Fructus were basically divided into 3 groups by cluster analysis and principal component analysis, which were consistent with the classification of three different producing areas. Eight differential markers were screened by orthogonal partial least squares discriminant analysis and four of them (5,7-dimethoxycoumarin, bergapten, 6,7-dimethoxycoumarin and diosmin) were identified by reference substances. Similarity evaluation of 5 species of decoction pieces from genus <italic>Citrus</italic> in the family Rutaceae was carried out by taking the reference fingerprint of Citri Sarcodactylis Fructus as treference chromatogram, similarity of Citri Sarcodactylis Fructus decoction pieces was 0.892-0.977, and the similarities of the other 4 kinds of decoction pieces were 0.215-0.517. Conclusion:The established fingerprint method is reasonable, effective and accurate for quality control of Citri Sarcodactylis Fructus, the characterization information is more comprehensive combined with chemometrics.

11.
Journal of Medical Biomechanics ; (6): E096-E101, 2021.
Article in Chinese | WPRIM | ID: wpr-904371

ABSTRACT

Objective To establish the three-dimensional (3D) statistical shape model (SSM) of the foot, so as to reveal the 3D foot shape variations. Methods Foot data from 50 normal Chinese young males were used for 3D statistical shape modelling. Steps, including mesh registration of foot surface, axis alignment and principal component (PC) analysis (dimension reduction), were performed to obtain the parameterized foot shape (mean shape and standard deviation of PC). Results Through the principal component analysis (PCA), the 3D foot shape varied in the length and width (PC1, 48.01%), arch and dorsal height (PC2, 11.38%), and hallux abduction-adduction position (PC3, 7.48%). Conclusions Based on the parameterised 3D foot SSM, these datasets can be applied into the population-based shoe last manufacture, orthotics customization and quick diagnosis of foot disorders in clinic.

12.
Article in Chinese | WPRIM | ID: wpr-906325

ABSTRACT

Objective:To establish the ultraperformance liquid chromatography (UPLC) fingerprint of Pipa Qingfeiyin substance benchmark, and to establish a quantitative analysis method for simultaneous determination of the contents of five index components, so as to provide reference for the quality control and evaluation of this famous classical formula. Method:ACQUITY UPLC<sup>®</sup> CSH<sup>TM</sup> C<sub>18</sub> column (2.1 mm×100 mm, 1.7 μm) was used with mobile phase of acetonitrile (A)-0.1% formic acid aqueous solution (B) for gradient elution (0-7 min, 5%-7%A; 7-11 min, 7%-8%A; 11-22 min, 8%-14%A; 22-30 min, 14%-15%A; 30-35 min, 15%-25%A; 35-42 min, 25%-40%A; 42-45 min, 40%-50%A; 45-50 min, 50%-60%A), the flow rate was 0.35 mL·min<sup>-1</sup>, the column temperature was 25 ℃, the detection wavelengths were 278 nm and 248 nm. UPLC fingerprints of 15 batches of Pipa Qingfeiyin substance benchmark were established, and the "Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine" software (2012 edition) was used for similarity analysis, and the common peaks were assigned. Cluster analysis (CA), principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) were used to evaluate the fingerprint data. UPLC fingerprint method was used to simultaneously determine the contents of five components in the substance benchmark. Result:The method validation of fingerprint and determination method was good, the similarities between 15 batches of Pipa Qingfeiyin substance benchmark and their control fingerprint were ≥0.997, 23 common peaks were identified and 11 chromatographic peaks were identified. CA, PCA and OPLS-DA divided 15 batches of the substance benchmark into two groups. The linear relationship of phellodendrine hydrochloride, chlorogenic acid, berberine hydrochloride, palmatine hydrochloride and ammonium glycyrrhizinate was good in a certain range of concentration (<italic>R</italic><sup>2</sup>>0.999), their average recovery was 96.47%-101.16%, and the contents of these five components in the substance benchmark were 0.87-2.00, 1.53-5.95, 18.45-33.97, 3.87-6.29, 1.02-4.12 mg·g<sup>-1</sup>, respectively. Conclusion:The established UPLC fingerprint and multi-index component content determination methods have strong specificity, good resolution and high sensitivity, it can be characterized except for the Ginseng Radix et Rhizoma flavor, which can provide reference for the quality control and evaluation of Pipa Qingfeiyin compound preparation.

13.
Article in Chinese | WPRIM | ID: wpr-846400

ABSTRACT

Objective: To establish a method for the identification of the Periplaneta americana and other insectivorous herbs (Scorpio and Hirudo) based on infrared spectroscopy combined with chemometrics, and to provide a basis for the identification of the P. americana. Methods: Fourier transform infrared spectroscopy was used to collect the infrared spectrum data of three kinds of insect medicine powders. After the second order derivation of the obtained spectral data, the ordinate verticalization method and standardization method were used to optimize the spectrum. The spectral data was further analyzed by chemometrics, such as hierar chicalcluster analysis (HCA), principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). Results: There were differences in the infrared fingerprints of the P. americanas, Scorpios, Leeches. The absorption peaks of the P. americanas at 1 711, 1 410, and 712 cm-1 were obvious. The absorption peaks of the Scorpios at 1 753, 1 400, 1 168, and 717 cm-1 were obvious. The absorption peaks of the Leeches at 1 558, 1 457, 1 400, and 669 cm-1 were obvious, And the leeches have no absorption peak at 1 753-1 711 cm-1. The peak shape of the three insectivorous herbs was significantly different at 1 800-1 700 cm-1. In the second derivative spectrum, the positions of the main peaks are the same, but the intensity of the common peaks is different. Using the HCA analysis method, it was found that the three insectivorous herbs could be quickly distinguished. The PCA and PLS-DA analysis methods were used to find that the three insectivorous herbs were distributed in different regions. Conclusion: Infrared spectroscopy combined with chemometrics can easily and quickly identify the P. americanas and other insectivorous herbs (Scorpios and Leeches), and provide reference for the quality control and evaluation of P. americanas.

14.
Article in Chinese | WPRIM | ID: wpr-845184

ABSTRACT

Objective: To analyze and compare the volatile components of Jiuwei Qianghuo pills, granules and oral liquid. Methods: The volatile components of Jiuwei Qianghuo pills, granules and oral liquid were analyzed and compared by the head-space solid-phase microextraction and gas chromatography-mass spectrometry(HS-SPME-GC-MS), the relative percentage of each component was calculated using the area normalization method, and the principal component analysis was also performed. Results: A total of 90 kinds of volatile components were identified from Jiuwei Qianghuo pills, accounting for 97.19% of the total volatile components; 27 kinds of volatile components were identified from Jiuwei Qianghuo granules, accounting for 92.92% of the total volatile components;22 kinds of volatile components were identified from Jiuwei Qianghuo oral liquid, accounting for 87.60% of the total volatile components. A total of 111 volatile components were identified in the three preparations, of which 6 were common components, but the contents of the common components were different. The specific components of the pills, granules and oral liquid were 68, 8 and 13, respectively. Moreover, the comprehensive scores of the three dosage forms in the principal component analysis showed a large difference, with the high, middle and low values for the pills, granules and oral liquid, respectively. Conclusion: The composition and content of volatile components were different in the Jiuwei Qianghuo pill, granule and oral liquid preparations. From the point of view of the volatility, the comprehensive score of Jiuwei Qianghuo pills is higher than that of granules and oral liquid.

15.
Article in Chinese | WPRIM | ID: wpr-872901

ABSTRACT

Objective:High performance liquid chromatography (HPLC) fingerprints of liposoluble and water-soluble fractions of Xiaojinwan were established and the similarity of fingerprints was evaluated, so as to explore the quality consistency of Xiaojinwan. Method:Chromatographic separation was carried out on Welch Ultimate AQ-C18 column (4.6 mm×250 mm, 5 μm) with the mobile phase of 0.1% phosphoric acid solution (A)-acetonitrile (B) for gradient elution (liposoluble fraction of 0-5 min, 40%B; 5-10 min, 40%-50%B; 10-20 min, 50%-60%B; 20-30 min, 60%-65%B; 30-40 min, 65%-70%B; 40-50 min, 70%-80%B; 50-60 min, 80%-90%B; 60-65 min, 90%-95%B; 65-75 min, 95%-100%B; 75-80 min, 100%B; water-soluble fraction of 0-20 min, 2%-5%B; 20-30 min, 5%-10%B; 30-37 min, 10%-20%B; 37-45 min, 20%-30%B; 45-50 min, 30%-40%B; 50-58 min, 40%B), the flow rate was 1 mL·min-1, the column temperature was 30 ℃. The detection wavelengths of the liposoluble and water-soluble fractions were 202, 250 nm, and their injection volumes were 10, 20 μL, respectively. A total of 30 batches of Xiaojinwan from five manufacturers were detected by HPLC, the chromatographic peaks of each part were analyzed by principal component analysis (PCA) and identified. Result:A total of 55 chromatographic peaks were detected in the fingerprints, and the similarity of fingerprint of 30 batches of Xiaojinwan was quite different. The relative standard deviations (RSDs) of fingerprint similarity of liposoluble and water-soluble fractions of Xiaojinwan were 21.5% and 32.8%, respectively. There were significant differences in the quality of samples from different manufacturers and the same manufacturer, and the chemical consistency evaluation results were dominated by liposoluble fraction, and the main reason for the chemical difference of this preparation was the composition of Liquidambaris Resina. Conclusion:The quality consistency of Xiaojinwan is poor. The establishment of two-fraction fingerprint provides a new idea for the overall quality evaluation and control of Xiaojinwan, and can provide a reference for the quality consistency evaluation of traditional pills.

16.
Article in Chinese | WPRIM | ID: wpr-873066

ABSTRACT

Objective:To compare the effects of different processing techniques on the chemical constituents of Aurantii Fructus for screening the dominant decoction pieces. Method:UPLC-Q/TOF-MS was used to detect the chemical constituents of Aurantii Fructus, chromatography separation was achieved on an ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm), and gradient elution was performed with 0.1% formic acid aqueous solution (A)-0.1% formic acid acetonitrile solution (B) as mobile phase (0-10 min, 5%-35%B; 10-18 min, 35%-75%B; 18-21 min, 75%-100%B; 21-24 min, 100%B; 24-24.1 min, 100%-5%B; 24.1-28 min, 5%B). Data acquisition was carried out in electrospray ionization (ESI) under the positive ion mode, the scanning range was m/z 50-1 200. The chemical constituents in methanol extract of Aurantii Fructus were identified according to reference substance, relative molecular weight, mass spectrometric cleavage rule and literature information. SIMCA-P 13.0 software was used to establish principal component analysis (PCA) model and partial least squares-discriminant analysis (PLS-DA) model of Aurantii Fructus processed products, PCA score plot, PLS-DA loading plot and variable importance in the protection (VIP) values were obtained to screen the material basis for the main differences before and after processing of Aurantii Fructus. Result:A total of 54 chemical components were identified by UPLC-Q/TOF-MS. PCA indicated that there were significant differences among different groups of Aurantii Fructus processed by different methods. A total of 14 chemical components with VIP value >1 were screened by PLS-DA as the main chemical markers for the differences before and after processing, including hesperidin, poncirin, narirutin, etc. The comprehensive weighted score showed that the content of effective components in Aurantii Fructus processed with honey bran was the highest. Conclusion:The contents of chemical constituents in Aurantii Fructus before and after processing are significantly changed. Flavonoids are the most important compounds to distinguish different processed products of Aurantii Fructus. Aurantii Fructus processed with honey bran is the dominant variety.

17.
Article in Chinese | WPRIM | ID: wpr-873030

ABSTRACT

Objective:To improve the quality standard of Shenwei Gubi tablets, and to explore the reasons for the great difference in the contents of quality control index components between batches of this product. Method:The fingerprint of this product was established by HPLC, the determination was performed on Diamonsil C18 column (4.6 mm×250 mm, 5 μm) with acetonitrile (A)-0.1% phosphoric acid solution (B) for gradient elution (0-5 min, 10%A; 5-15 min, 10%-12%A; 15-30 min, 12%-26%A; 30-43 min, 26%-31%A, 43-50 min, 31%-40%A, 50-70 min, 40%-55%A; 70-84 min, 55%-72.5%A) as the mobile phase at detection wavelength of 230 nm. The orthogonal partial least squares-discriminant analysis-variable importance in the projection (OPLS-DA-VIP) map was drawn with the common peak as the independent variable. The contribution of 26 common peaks to the fingerprint differences among different batches of this product was quantified. By searching for the chromatographic peaks with great differences, combined with relevant literature, the components related to the clinical indications of the product were screened out and their contents were determined by specificity experiment, and the quantitative indicators were finally selected. HPLC-doide array detector (DAD) was employed to determine the contents of the above preferred indexes with detection wavelengths of 236, 276, 230, 322 nm, other conditions were the same as HPLC fingerprint detection method. Result:A total of 26 common peaks were calibrated on the HPLC fingerprint of Shenwei Gubi tablets. The similarity between the fingerprint of each batch samples and the reference fingerprint was≥0.950. Loganic acid, gentiopicroside, paeoniflorin and osthole were optimized as the quantitative indicators of this product, their average contents were 161.02, 401.80, 255.54, 80.68 μg·g-1. Conclusion:The established fingerprint and multi-index quantitative analysis method are stable and reliable, and can be used for quality control of Shenwei Gubi tablets. Difference in contents of quality control components between batches of raw materials and the imperfect quality control method of intermediates in the production process are the main reasons for the great difference in the contents of quality control indicators between batches of this product.

18.
Article in English | WPRIM | ID: wpr-847075

ABSTRACT

Background: With increasing media coverage of food safety incidents, such as that of clenbuterol residues in pork, food safety has become a major public health concern in China. Rapidly developing online markets attract increasing numbers of Chinese consumers to purchase food on the Internet. However, the quality and safety of food sold online are uncertain and are less reported on. Objective: This research aimed to systematically study the quality and safety of chilled pork from wet markets, supermarkets, and online markets in China. Results: The chilled pork samples from online markets were fresher than those from wet markets and supermarkets based on the surface redness (a* value). Chilled pork contained high levels of nutritional elements, especially the magnesium and phosphorus levels in samples from online markets. The levels of heavy metal element residues and veterinary drug residues in all chilled pork samples were within the standards limits. In addition, huge differences existed in the quality and freshness of the chilled pork samples from online markets according to principal component analysis (PCA). Conclusions: Most chilled pork sold in Chinese markets was qualified and safe. It is necessary to establish an effective online market supervision system for chilled pork.

19.
Chinese Herbal Medicines ; (4): 406-411, 2019.
Article in Chinese | WPRIM | ID: wpr-842052

ABSTRACT

Objective: Poria cocos and Polyporus umbellatus are similar medicinal fungi in traditional Chinese medicines. A method for fingerprint analysis of monosaccharide composition of polysaccharides by HPLC combined with chemometrics methods has been developed for characterization and discrimination of them in this research. Methods: The polysaccharides were extracted by decocting in water, and then completely hydrolyzed with hydrochloride. Monosaccharides in the hydrolyzates were derivatized with 1-phenyl-3-methyl-5-pyrazolone (PMP) for HPLC analysis. More than 20 batches of P. cocos and P. umbellatus from different regions were analyzed. Results: The fingerprints of P. cocos showed five common characteristic peaks, which were identified by comparing with the reference substances. The five peaks corresponded to the derivatives of mannose, ribose, glucose, galactose, and fucose. At the same time, the fingerprints of P. umbellatus showed eight common characteristic peaks, of which seven were identified as the derivatives of mannose, ribose, rhamnose, glucose, galactose, xylose, and fucose. Moreover, the similarity of their fingerprints was respectively calculated by the Similarity Evaluation System for Chromatographic Fingerprint of TCM published by China Pharmacopoeia Committee (Version 2004A). And the data were further processed by hierarchical cluster analysis (HCA) and principal component analysis (PCA). The similarity evaluation and HCA indicated that there were no significant difference in P. cocos or P. umbellatus samples from different geographical regions, but PCA was performed to characterize the difference in monosaccharide constituents between P. cocos and P. umbellatus, and linear discriminant analysis (LDA) showed the overall correct classification rate was 100%. Conclusion: The fingerprint analysis method of monosaccharide composition of water-soluble polysaccharides can distinguish P. cocos and P. umbellatus, and can be applied for the authentication or quality control for P. cocos and P. umbellatus.

20.
Article in Chinese | WPRIM | ID: wpr-350211

ABSTRACT

To compare the differences of main components between in rhizoma and fibrous root of Trillium tschonoskii and T. kamtschaticum, a simple, accurate and reliable high performance liquid chromatography coupled with the charged aerosol detector (HPLC-CAD) method was developed and then successfully applied for simultaneous quantitative analysis of three compounds, including polyphyllin Ⅶ (T1),pennogenin 3-O-α-L-rhamnopyranosyl-(1→2) [α-L-rhamnopyranosyl-(1→4)]-β-D-glucopyranoside (T2),polyphyllin Ⅵ (T3), in 16 batches of rhizome and 14 batches of fibrous root. The analytes were well separated from other constituents on TSK gel ODS (4.6 mm×250 mm, 5 μm) with acetonitrile-water (43∶57) at a flow rate of 1.0 mL•min⁻¹. The injection volume was 20 μL. The nitrogen inlet pressure for the CAD system was 35 psi and the nebulizer chamber temperature was 35 ℃.The method was validated for linearity (r>0.999 0), intra and inter-day precision (0.29%-3.0%), repeatability (0.45%-1.4%), stability (1.9%-2.6%), recovery (100.1%-100.2%, 1.2%-1.8%), limits of detection (0.002 g•L⁻¹), and limits of quantification (0.005 g•L⁻¹).The obtained datasets were processed by principal component analysis (PCA) and it showed that there was almost no difference in rhizoma of T. tschonoskii and T. kamtschaticum from different areas of China. However, the 3 major compounds existed in rhizoma were different from those in fibrous root of T. tschonoskii and T. kamtschaticum.

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