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1.
Article in Chinese | WPRIM | ID: wpr-906467

ABSTRACT

Objective:The differences of chemical compositions and pharmacological activities between the core and pulp of Phyllanthi Fructus were investigated by chemical analysis and <italic>in vitro</italic> test to explore the effect of the core on the quality of this medicinal material. Method:Literature, medicinal material standards and market research on the appearance of Phyllanthi Fructus were conducted based on existing databases. Ultra-high performance liquid chromatography-quadrupole-electrostatic field orbital trap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) was used to identify the constituents of the core and pulp. The analysis was performed on Thermo Scientific Accucore C<sub>18</sub> column (2.1 mm×100 mm, 2.6 μm) with the mobile phase of 0.1% formic acid aqueous solution (A)-methanol (B) for gradient elution (0-25 min, 5%B; 25-30 min, 5%-95%B; 30-35 min, 95%-5%B), the flow rate was 0.2 mL·min<sup>-1</sup>, heating electrospray ionization (HESI) was adopted with positive and negative ion modes, and the scanning range was <italic>m</italic>/<italic>z</italic> 100-1 500. High performance liquid chromatography (HPLC) was used to determine the contents of gallic acid, corilagin, chebulagic acid and ellagic acid in the core and pulp of Phyllanthi Fructus. Analysis was performed on Welchrom C<sub>18</sub> column (4.6 mm×250 mm, 5 μm) with mobile phase of methanol (A)-0.05% phosphoric acid aqueous solution (B) for gradient elution (0-6 min, 5%A; 6-15 min, 5%-7%A; 15-20 min, 7%-15%A; 20-25 min, 15%-21%A; 25-31 min, 21%-22%A; 31-41 min, 22%A; 41-47 min, 22%-28%A; 47-51 min, 28%-32%A; 51-57 min, 32%-38%A; 57-70 min, 38%-45%A; 70-80 min, 45%-65%A; 80-85 min, 65%-5%A), the detection wavelength was set at 270 nm. The antibacterial effects of the core and pulp of Phyllanthi Fructus on <italic>Escherichia coli</italic> and <italic>Staphylococcus aureus</italic> were investigated by filter paper method, and their antioxidant activities were compared by 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging assay. Result:A total of 47 compounds were identified in the core and pulp of Phyllanthi Fructus, mainly including tannins, flavonoids, phenolic acids, fatty acids, amino acids, organic acids, saccharides and glycosides, most of which were concentrated in the pulp, and the fatty acids in the core accounted for a higher proportion. The contents of gallic acid, corilagin, chebulagic acid, ellagic acid and other phenolic compounds in the pulp of 20 batches of Phyllanthi Fructus were much higher than those in the core. The results of antibacterial test showed that the core of Phyllanthi Fructus with different concentrations had no antimicrobial effect. The DPPH radical scavenging test showed that the antioxidant activity of the core [half-inhibitory concentration (IC<sub>50</sub>)=199.632 mg·L<sup>-1</sup>] was much less than that of the pulp (IC<sub>50</sub>=12.688 mg·L<sup>-1</sup>). Conclusion:From the perspectives of polyphenol content, antibacterial and antioxidant activities, it is scientific to use Phyllanthi Fructus pulp in ancient and modern times, which may be to remove the secondary parts of Phyllanthi Fructus, so as to enhance the actual utilization rate and therapeutic effect of medicinal materials. In view of the large proportion of the core of Phyllanthi Fructus and its high content of fatty acids and other components, whether or not to use it remains to be further studied in clinical application.

2.
Article in Chinese | WPRIM | ID: wpr-906466

ABSTRACT

Objective:To establish a high performance liquid chromatography (HPLC) fingerprint of branches of <italic>Juglans mandshurica</italic> and to evaluate the quality of the samples from different producing areas and in different harvest periods. Method:Chromatographic separation was performed on an Agilent Poroshell 120 SB-C<sub>18</sub> column (2.1 mm×100 mm, 2.7 μm) for gradient elution with mobile phase of 0.2% formic acid solution (A)-0.2% formic acid acetonitrile solution (B) (0-5 min, 5%-10%B; 5-25 min, 10%-16%B; 25-40 min, 16%-22%B; 40-45 min, 22%-45%B; 45-50 min, 45%-65%B; 50-52 min, 65%-100%B; 52-55 min, 100%B) at a flow rate of 0.3 mL·min<sup>-1</sup>. The column temperature was 30 ℃ and the detection wavelength was 270 nm. The quality of branches of <italic>Juylans mandshurica</italic> was evaluated by similarity evaluation, cluster analysis, principal component analysis and partial least squares-discriminant analysis. The chemical constituents of the samples were identified by HPLC coupled with quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS/MS). The mass spectrometry was conducted in negative ion mode with electrospray ionization(ESI). Data were acquired over a range of <italic>m</italic>/<italic>z</italic> 100-1 700 for MS and <italic>m</italic>/<italic>z</italic> 50-1 700 for MS/MS. Result:A total of 19 common peaks were confirmed in 40 batches of samples, and the similarity ranged from 0.430 to 0.995, of which the similarity of samples collected in spring and winter seasons (April, May and December) was greater than 0.90, while the similarity of most samples collected in summer (July to September) was low. Multivariate statistical analysis showed that the samples were divided into two groups according to the harvest time, but there was no obvious classification rule for the samples from different producing areas. The contents of most constituents in the samples collected in spring and winter were higher than those collected in summer. The result illustrated that different harvest periods had great influence on the quality of branches of <italic>J</italic>.<italic> mandshurica</italic>. Compared with the samples collected in summer, the quality of samples collected in spring and winter was better. A total of 22 peaks were proved to be the main constituents that contributed to the difference between samples collected in different seasons. A total of 83 chemical components were identified by HPLC-Q-TOF-MS/MS, including 49 tannins, 7 organic acids, 14 naphthalene derivatives, 1 flavonoid, 6 anthracene derivatives, 2 lignans, 3 diarylheptanoids and 1 saccharide. Totally 13 common peaks were identified. Of the peaks that contributed to discriminate samples collected in different season, 19 peaks were identified and most of them were tannins. Conclusion:The established HPLC fingerprint can provide useful information for the quality evaluation of branches of <italic>J</italic>.<italic> mandshurica</italic>. Tannin is the main constituents in the samples. Harvest period has great influence on the quality of branches of <italic>J</italic>.<italic> mandshurica</italic>.

3.
Article in Chinese | WPRIM | ID: wpr-906217

ABSTRACT

Objective:Through comprehensive evaluation and analysis of the quality of Liuwei Dihuang (LWDH) preparations from different manufacturers and combining factors such as production technology, the key factors in the quality control of LWDH preparations are explored to provide a reference for improving the quality control level of LWDH preparations. Method:Morroniside, loganin and paeonol as quality control markers of LWDH products were determined by high performance liquid chromatography (HPLC), the mobile phase was acetonitrile (A) -0.3% phosphoric acid aqueous solution (B) for gradient elution (0-5 min, 5%-8%A; 5-20 min, 8%A; 20-35 min, 8%-20%A; 35-45 min, 20%-60%A; 45-55 min, 60%A), the detection wavelength of paeonol was at 274 nm, and the detection wavelengths of morroniside and loganin were at 240 nm. The quality characteristics of LWDH preparations with different dosage forms (big candied pills, water-honeyed pills, concentrated pills, hard capsules and soft capsules) from different manufacturers were analyzed. Combined these results with their actual production processes, the key-points of quality control in the whole production process were discussed. Result:The contents of three index ingredients in 128 batches of LWDH preparations were all in conformity with the standards of the 2015 edition of <italic>Chinese Pharmacopoeia</italic>, however, the content limit of some dosage forms in the current standard was unreasonable. For example, although the daily dose of crude drugs for big candied pills were almost twice the dose of water- honeyed pills (15.00, 8.57 g, respectively), they got exactly the same daily limits of the contents for both the quality markers. What′s more, these two formulations had the same process, so the differences between the process obviously could not be the reason of these differences. Conclusion:It is recommended that for the products with different dosage forms should have a similar content limits, if there are no obvious distinctions between their production processes. Which may benefit the quality control of the products with multi-dosage forms. The research on the quality standards of proprietary Chinese medicines should deeply study the existing characteristics of the quality standards, and fully respect the laws of the quality attributes of traditional Chinese medicines and the rules of the production process of Chinese patent medicines.

4.
Article in Chinese | WPRIM | ID: wpr-906139

ABSTRACT

Objective:To explore the quality transmitting relationship between decoction pieces and substance benchmarks with the fingerprint, index component content and dry extract rate as evaluation indexes, and investigate the key quality attributes of 15 batches of substance benchmarks of Yihuangtang, and establish the quality standard of this substance benchmarks. Method:Fifteen batches of Yihuangtang substance benchmarks freeze-dried powder samples were prepared, the fingerprint and index component content of 15 batches of decoction pieces and substance benchmarks were determined by high performance liquid chromatography (HPLC), the mobile phase was acetonitrile (A)-0.1% phosphoric acid aqueous solution (B) for gradient elution (0-6 min, 97%B; 6-12 min, 97%-92%B; 12-25 min, 92%-90%B; 25-35 min, 90%-89%B; 35-50 min, 89%-82%B; 50-75 min, 82%-72%B; 75-85 min, 72%-35%B), the detection wavelength was set at 230 nm, combined the dry extract rate to clarify the attribution of characteristic peaks and the range of similarity with the control chromatogram, the content range and transfer rate range of geniposidic acid and berberine hydrochloride, the dry extract rate range and the variation range of the substance benchmarks. Result:The established HPLC fingerprint had good precision, repeatability and stability, and could be used for the simultaneous determination of decoction pieces and substance benchmarks of Yihuangtang. The similarities between the control chromatogram and fingerprint of substance benchmarks were >0.99. A total of 15 characteristic peaks were assigned, and 8 characteristic peaks were identified by the reference substances, of which 6 were from Phellodendri Chinensis Cortex processed with salt, 1 was from Plantaginis Semen processed with wine, and 1 was from stir-fried Dioscoreae Rhizoma. The content ranges of geniposidic acid and berberine hydrochloride in 15 batches of substance benchmarks of Yihuangtang were 0.10%-0.16% and 0.63%-1.05%, the transfer rate ranges of them were 20.91%-32.65% and 19.60%-29.59%, respectively. The dry extract rate range of the substance benchmarks was 8.45%-9.92%. Conclusion:The quality standard of Yihuangtang substance benchmarks can be preliminarily formulated by the combination of fingerprint, dry extract rate and determination of index component, which can provide the basis for the quality control of Yihuangtang and the development of related preparations.

5.
Article in Chinese | WPRIM | ID: wpr-906121

ABSTRACT

Objective:To evaluate the scientificity and feasibility of processing of Pinelliae Rhizoma by hot water washing (Tangxi), and to provide reference for the development of related famous classical formulas. Method:Processing method of Pinelliae Rhizoma washed by hot water was established based on ancient Tangxi processing method, and the process conditions were optimized by single factor tests. The weight, moisture, ash, extract, total acid (calculated by succinic acid) contents and high performance liquid chromatography (HPLC) fingerprint of Pinelliae Rhizoma were compared before and after processing. In addition, the rabbit eye irritation test was conducted to evaluate the toxicity changes. Result:The processing method of Pinelliae Rhizoma washed by hot water was as following:washed by 4 times the amount of hot water at 80 ℃ for 10 times until clear water, transfused cross-section after incision, no or slight numbness in the mouth. The average moisture, ash, extract contents of Pinelliae Rhizoma washed by hot water were 9.34%, 1.71% and 4.22%, respectively. After being processed, the decline rates of weight and total acid content of Pinelliae Rhizoma were 7.49% and 43.31%. The HPLC fingerprint of Pinelliae Rhizoma before and after washing showed a decrease in all components, but there was no new chromatographic peak, and peak 9 (adenosine) reduced significantly. The results of rabbit eye irritation test showed that there was no obvious eye conjunctival irritation after washing, indicating that the toxicity of Pinelliae Rhizoma decreased obviously after washing. Conclusion:The established method of Pinelliae Rhizoma by Tangxi processing is stable and feasible, the aqueous extract of Pinelliae Rhizoma has no obvious eye conjunctival irritation after washing.

6.
Article in Chinese | WPRIM | ID: wpr-906063

ABSTRACT

Objective:The correlation between the appearance color of cooked rhubarb samples and the components characterized by high performance liquid chromatography (HPLC) fingerprint was studied to reveal the quality transfer law in the steaming process of processed products with rice-wine. Method:The visual analyzer was used to analyze the change of the appearance color of cooked rhubarb sample powder at different processing time, the common components and their relative peak areas of processed products with rice-wine were identified by HPLC fingerprint, as well as multivariate statistics and Pearson correlation analysis were used to cluster, discriminate and analyze the appearance color and the component variables in HPLC fingerprint. Result:During the processing of cooked rhubarb, the <italic>a</italic><sup>*</sup> (red-green value) of sample powder had no obvious change, but the <italic>L</italic><sup>*</sup> (lightness value), <italic>b</italic><sup>*</sup><italic> </italic>(yellow-blue value) and <italic>E</italic><sup>*</sup><italic>ab </italic>(total chromaticity value) showed a decreasing trend, and the appearance color changed from bright to dark, from yellow to brown. A total of 46 chromatographic peaks in the fingerprint were identified at 254 nm and 280 nm, and 18 of them were identified by comparison with reference standards. The change trend of <italic>L</italic><sup>*</sup>,<italic> b</italic><sup>*</sup><italic> </italic>and <italic>E</italic><sup>*</sup><italic>ab </italic>were positively correlated with the contents of tannins (catechin, epicatechin and ethyl gallate), stilbene glycoside (<italic>trans</italic>-3,5,4′-trihydroxystyryl-4′-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-glucoside), phenylbutanone glycoside of 4′-hydroxyphenyl-2-butanone-4′-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-[2ʺ-<italic>O</italic>-gallic-6ʺ-<italic>O</italic>-(4ʺ-hydroxy)-cinnamoyl)-glucoside, conjugated anthraquinones (aloe emodin-8-<italic>O</italic>-glucoside, rhein-8-<italic>O</italic>-glucoside, emodin-8-<italic>O</italic>-glucoside) and <italic>ω</italic>-hydroxyemodin (<italic>P</italic><0.05, <italic>P</italic><0.01), and negatively correlated with the contents of free anthraquinones (emodin, aloe emodin and physcion). Compared with 254 nm, the similarities of chromatographic peaks at 280 nm was more obvious, and the number of detected common peaks was more, which could reflect more subtle differences in chemical composition. Conclusion:Tannins, stilbene glycosides and phenylbutanone glycosides are strongly correlated with <italic>L</italic><sup>*</sup>, while anthraquinones are strongly correlated with <italic>b</italic><sup>*</sup>, the decrease of <italic>E</italic><sup>*</sup><italic>ab</italic> is mainly related to the increase of free anthraquinone content and the decrease of catechins, <italic>ω</italic>-hydroxyemodin, stilbene glycosides, conjugated anthraquinone and phenylbutanone glycosides. The change of appearance color index of process samples can reflect the change trend of the contents of medicinal components in cooked rhubarb to some extent.

7.
Article in Chinese | WPRIM | ID: wpr-905982

ABSTRACT

Objective:To establish high performance liquid chromatography (HPLC) fingerprint and multi-component determination for the substance benchmark of Yiweitang, and to evaluate its quality in combination with chemical pattern recognition method. Method:Fifteen batches of substance benchmark of Yiweitang were prepared, the "Chinese medicine chromatographic fingerprint similarity evaluation system" (2012 edition) was used to calculate similarity. Cluster analysis, principal component analysis and orthogonal partial least squares-discriminant analysis were employed to handle the common peaks for evaluating the quality difference among 15 batches of the substance benchmark. The contents of catalpol, verbascoside and methylophiopogonanone A were determined with mobile phase system of acetonitrile-phosphoric acid solution at detection wavelengths of 210 nm and 334 nm. Result:There were 22 common peaks in HPLC fingerprint of the substance benchmark, among them, peaks 1, 9, 12, 14-17, 19 and 20 belonged to Rehmanniae Radix, peaks 3, 4, 6, 7 and 21 belonged to Glehniae Radix, peaks 5 and 22 belonged to Ophiopogonis Radix, peaks 2 and 18 belonged to Polygonati Odorati Rhiaoma, peak 8 was the common peak of Ophiopogonis Radix and Rehmanniae Radix, peak 10 was shared by Ophiopogonis Radix, Polygonati Odorati Rhiaoma<italic> </italic>and<italic> </italic>Rehmanniae Radix, peak 11 was the common peak of these four herbs, and peak 13 was shared by Polygonati Odorati Rhiaoma and Rehmanniae Radix. The similarities between HPLC fingerprints of 15 batches of the substance benchmark and the control fingerprint were all >0.90, the samples could be divided into four categories by three chemical pattern recognition methods. Quantitative analysis showed that the contents of catalpol, verbascoside and methylophiopogonanone A among 15 batches of samples ranged from 0.37% to 1.14%, 0.002% to 0.054% and 0.016% to 0.079%, respectively. Conclusion:The established fingerprint and determination for the substance benchmark of Yiweitang have good separation and high accuracy, which reflect the overall chemical composition characteristics of Yiweitang, and can provide experimental basis for the further development and quality control of the compound preparations of this famous classical formula.

8.
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.

9.
Article in Chinese | WPRIM | ID: wpr-905951

ABSTRACT

Objective:Based on fingerprint, index component content and dry extract yield, a quality evaluation method for substance benchmark of Xiebaisan was established to study the key quality attributes, to explore the quantitative transfer relationship between decoction pieces and substance benchmark, and to preliminarily formulate the quality standard of substance benchmark of Xiebaisan. Method:The substance benchmark of Xiebaisan was prepared according to the records of ancient formulas, fingerprints of 15 batches of decoction pieces and substance benchmarks were collected by high performance liquid chromatography (HPLC) and the index components were determined with the mobile phase of acetonitrile-0.05% phosphoric acid solution for gradient elution. The dry extract yield, fingerprint similarity and transfer rate of index components were combined to study the quantity value transmitting. Result:Ten characteristic peaks were identified in fingerprint of the substance benchmark and two characteristic peaks from stir-fried Mori Cortex, four characteristic peaks from baked Lycii Cortex, four characteristic peaks from Glycyrrhizae Radix et Rhizoma Praeparata cum Melle. Mulberroside A, liquiritin and glycyrrhizic acid were used as index components for the determination, the contents of mulberroside A, liquiritin and glycyrrhizic acid in substance benchmark of Xiebaisan were 2.69%-4.26%, 0.09%-0.17% and 0.09%-0.16%, and their transfer rates were (31.37±4.14)%, (36.12±4.03)% and (12.25±0.88)%, respectively. The similarity of fingerprint of substance benchmarks was good, the fingerprint similarities of 14 batches of substance benchmarks and control fingerprint were >0.9. The dry extract yield of substance benchmark of Xiebaisan ranged from 8.09% to 11.29%. Conclusion:The established quality evaluation method of substance benchmark of Xiebaisan is scientific and reasonable, and the transfer process of decoction pieces to substance benchmarks is stable and controllable. The preliminary quality standard of the substance benchmark can provide basis and reference for the development of modern preparations of Xiebaisan in the future.

10.
Article in Chinese | WPRIM | ID: wpr-905910

ABSTRACT

Objective:Aiming at the residue of Shaoyao Gancaotang, the extraction, qualitative and quantitative study of the small molecule resource components were carried out to clarify the residual small molecule chemical components in the residue and explore the ways of its resource utilization. Method:The ultra-performance liquid chromatography-quadrupole-time-of-flight tandem mass spectrometry (UPLC-QTOF-MS/MS) was used to qualitatively identify the residual small molecule substances in the dregs of Shaoyao Gancaotang. Agilent C<sub>18</sub> reversed-phase chromatographic column (3.0 mm×100 mm, 2.7 µm) was used at the flow rate of 0.4 mL·min<sup>-1</sup>, the injection volume was 5 µL, and the mobile phase was gradient eluted with 0.05% formic acid aqueous solution (A)-acetonitrile (B) (0-1 min, 14%-17.5%B; 1-3 min, 17.5%-19%B; 3-4 min, 19%-20%B; 4-5 min, 20%B; 5-6 min, 20%-21%B; 6-9 min, 21%B; 9-22 min, 21%-36%B; 22-23 min, 36%B; 23-32 min, 36%-43%B), electrospray ionization (ESI) was employed with negative ion mode scanning and scanning range of <italic>m</italic>/<italic>z</italic> 50-1 200. A high performance liquid chromatography (HPLC) was established for the quantitative analysis of its main components with Agilent C<sub>18</sub> reversed-phase chromatographic column (4.6 mm×150 mm, 5 µm), the detection wavelength was set at 235 nm, the flow rate was 0.8 mL·min<sup>-1</sup>, and the injection volume was 5 µL. Mobile phase was 0.05% phosphoric acid (A)-acetonitrile (B) for gradient elution (0-1 min, 14%-19%B; 1-4 min, 19%B; 4-18 min, 19%-50%B). The content changes of main components in the residue of Shaoyao Gancaotang were compared before and after two different techniques of organic solvent extraction and enzymatic extraction. Result:A total of 16 chemical components in the residue of Shaoyao Gancaotang were qualitatively analyzed, and quantitative analysis found that there were many chemical components in the residue, among which the residues of 6 index components such as paeoniflorin and liquiritin reached more than 70% in the original decoction piece. After enzymolysis by cellulase, liquiritin in the residue could be converted into liquiritigenin. The content of crude polysaccharide in enzymatic extract of the residue was 6 times higher than that in the blank group, and the content was up to 12%. Conclusion:There are still many small molecule resource components in the residue of Shaoyao Gancaotang, which has great development potential. Organic solvents can be used to re-extract the target components in the residue, and liquiritin can be converted into liquiritigenin by biological fermentation technology, and the crude polysaccharide from the residue can be extracted by enzymatic method to develop animal feed. This study can provide reference basis and approach for reusing the residues of Shaoyao Gancaotang preparations and dispensing granules, so as to realize the high-value utilization of Shaoyao Gancaotang.

11.
Article in Chinese | WPRIM | ID: wpr-905905

ABSTRACT

Objective:According to the GB/T 15000.3-2008, to develop a fucosterol certified reference material based on the project approved by Standardization Administration. Method:Fucosterol was isolated from <italic>Laminaria japonica</italic> dried thallus via 95% ethanol extraction, vacuum concentration, repeated column chromatography separation, recrystallization in petroleum ether-ethyl acetate, and residual solvent removal. Its chemical structure was identified by elemental analysis (EA), infrared spectrum (IR), mass spectrometry (MS), nuclear magnetic resonance (NMR) and X-ray diffraction (XRD). Its homogeneity, stability, and cooperative certification conducted by 8 laboratories were carried out by high performance liquid chromatography with evaporative light scattering detector. Result:For the fucosterol reference material, the certified value of purity was 99.54% with expanded uncertainty of 0.16% in confidence interval of 95%, the stability was good within 24 months storage period at 2-4 ℃, which met the technical requirements of reference material and passed the acceptance organized by Standardization Administration. Conclusion:The national standard materials of fucosterol has been successfully developed, which can be used for the determination of this component, the evaluation of detection methods, and the detection and quality control of related products.

12.
Article in Chinese | WPRIM | ID: wpr-905842

ABSTRACT

Objective:To establish a high performance liquid chromatography (HPLC) fingerprint of the substance benchmark of Xiao Chengqitang and evaluate its quality with chemical pattern recognition method. Method:Diamonsil C<sub>18</sub> column (4.6 mm×150 mm, 5 μm) was used, mobile phase was consisted of methanol (A)-0.1% phosphoric acid solution (B) for gradient elution (0-60 min, 20%-90%A; 60-70 min, 90%-100%A), the flow rate was 1 mL·min<sup>-1</sup>, the column temperature was 25 ℃, and the detection wavelength was 254 nm. The similarity evaluation system of chromatographic fingerprint of traditional Chinese medicine (2012 edition) was used to evaluate the similarity of HPLC fingerprint of 15 batches of substance benchmark of Xiao Chengqitang, and the chromatographic data were analyzed by cluster analysis, principal component analysis and orthogonal partial least squares-discriminant analysis, in order to evaluate the quality difference between different batches of substance benchmarks of Xiao Chengqitang and find out the main chemical components that caused the quality difference. Result:The HPLC fingerprint of Xiao Chengqitang substance benchmarks was established, 31 common peaks were identified, and 18 components were identified by comparing with the reference substances. The similarities of 15 batches of HPLC fingerprint of Xiao Chengqitang substance benchmarks were >0.92. The samples could be divided into two categories by three chemical pattern recognition methods. Nine main components leading to the quality discrepancy of samples between batches were screened out, including rhein, chrysophanol-8-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-glucoside, aloe-emodin-8-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-glucoside, sennoside A, chrysophanol-1-<italic>O</italic>-<italic>β</italic>-<italic>D</italic>-glucoside, rhein-8-<italic>O</italic>-glucoside and others. Conclusion:The established fingerprint analysis method is accurate, stable and reproducible, which basically reflects the overall chemical composition characteristics of Xiao Chengqitang, and can be used for the quality control of Xiao Chengqitang preparations.

13.
Article in Chinese | WPRIM | ID: wpr-905839

ABSTRACT

Objective:To screen qualitative preparation quality markers of Yuliantang, in order to provide data support for the selection of indicator components, and establish the direct connection between indicator components and efficacy (Xiehuo Zhitong) for achieving the quantity-effect combination. Method:The stability of preparation process of Yuliantang lyophilized powder was investigated by HPLC fingerprint technology, then, the components in Yuliantang lyophilized powder were identified by UHPLC-LTQ-Orbitrap-MS. By referring to the relevant literature, the pharmacological activities of these identified compounds were compared with the pharmacological effects corresponding to the efficacy of Yuliantang, and the composition of the qualitative preparation quality markers of Yuliantang lyophilized powder was determined. Result:The similarities between HPLC fingerprint of 10 batches of Yuliantang lyophilized powder and the control fingerprint were >0.9, indicating that the preparation process was stable and feasible. A total of 29 components were identified from Yuliantang, of which 23 alkaloids, 3 phenylpropanoids, 2 sesquiterpenoids and 1 limonoid, and there were 15 ingredients of<italic> </italic>Coptidis Rhizoma, 12 ingredients of<italic> </italic>Euodiae Fructus, and 2 ingredients of<italic> </italic>Aucklandiae Radix. The composition of the qualitative preparation quality markers of Yuliantang was initially determined as magnoflorine or 10-hydroxy-2,3,9-trimethoxyberberine, phellodendrine, menisperine, thalifendine, groenlandicine, dehydroevodiamine, coptisine, jatrorrhizine, columbamine, methylcoptisine, berberine, epiberberine, palmatine, evodiamine, rutaecarpine, neochlorogenic acid, cryptochlorogenic acid, chlorogenic acid, limonin, costunolide, dehydrocostus lactone. Conclusion:The method for researching and screening the preparation quality markers in Yuliantang lyophilized powder is scientific, reasonable and feasible, it can provide reference for the determination of component indicators in the process research of Yuliantang and qualitative and quantitative indexes in its quality standard.

14.
Article in Chinese | WPRIM | ID: wpr-905057

ABSTRACT

Objective:Powders and decocted powders account for about 1/3 in the Catalogue of Ancient Famous Classical Formulas (the First Batch), and have a very important position. Determination of preparation technology and particle size in the pulverization process is the key step in the research and development of powders and decocted powders following the original methods. However, there are many terms describing the preparation technology and particle size of powders and decocted powders in ancient Chinese medical books, and the parameters are not clear. Due to the lack of unified basis of particle size, the existing research results have not formed a uniform consensus. Based on ancient textual researches and experimental results, this article discusses the particle size of decocted powders and powders. Method:Through textual researches of the preparation technology and particle size of powders and decocted powders and powder classification in the 2020 edition of Chinese Pharmacopoeia, the specifications of pulverized particle size were suggested. In addition, Xiebaisan and Danggui Buxuetang were taken as examples to investigate the influence of different particle sizes (4, 10, 24 mesh) on the preparation process of decocted powders and the obtained decoction. Result:The particle size of 4 mesh was equivalent to that of ancient as big as hemp bean. The contents of index components in Xiebaisan and Danggui Buxuetang with particle size of 4 mesh were higher than that of 10 mesh and 24 mesh, but the particle size of 50 mesh was too fine to be filtered. Conclusion:The suggested particle sizes of powders and decocted powders are recommended as Cumo is the power through 10-mesh sieve, Mo is the power through 24-mesh sieve, Ximo is the power through 80-mesh sieve, as big as hemp bean is the power through 4-mesh sieve and not through 10-mesh sieve.

15.
Organ Transplantation ; (6): 595-2021.
Article in Chinese | WPRIM | ID: wpr-886789

ABSTRACT

Objective To establish a detection system of ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for everolimus concentration in whole blood of liver transplant recipients. Methods The proteins of samples were precipitated with methanol and zinc sulfate, and everolimus-D4 was used as the internal standard. Phenomenex Kinetex PFP column was used. The mobile phase A was water (containing 2 mmol/Lammonium formate and 0.1% formic acid), and the mobile phase B was methanol (containing 2 mmol/L ammonium formate and 0.1% formic acid). The gradient elution was performed with the flow rate of 1 mL/min, the column temperature of 50 ℃ and the injection volume of 1 μL. The multi-reaction monitoring mode was used to quantitatively analyze with electrospray positive ionization. The UPLC-MS/MS detection system required only 100 μL of whole blood, and could achieve a sufficient lower limit of quantification without complicated sample preparation. The total running time was within 4.5 min. Linear regression (1/x2) analysis was performed using peak area of everolimus / peak area of everolimus-D4 (y) and concentration of everolimus/concentration of everolimus-D4 (x) to calculate the calibration function and analyze its accuracy and linear relationship. UPLC-MS/MS was used to detect the trough blood concentration of everolimus in blood samples of 5 recipients after liver transplantation. Results The accuracy of quality control was within 15%, and the linear relationship of everolimus was good in the blood concentration range of 1-100 ng /mL(R2 > 0.990). Trough blood concentration of everolimus measured in blood samples of 5 liver transplant recipients ranged from 3.77 to 9.27 ng/mL. Conclusions The detection system of UPLC-MS/MS in this study is suitable for monitoring the concentration of everolimus in whole blood of liver transplant recipients because of its high accuracy, simple sample processing method and short detection time.

16.
Article in Chinese | WPRIM | ID: wpr-876173

ABSTRACT

Objective:To establish a high performance liquid chromatographic(HPLC) quantitative method for the determination of polyaminopropyl biguanide(PAPB) in cosmetics. Methods:Different forms of cosmetic samples were prepared by ultrasonic extraction and followed by high speed centrifugation of the extraction solution. The supernatant was degreased by hexane, and then was filtered by 0.22 μm millipore filter. The continued filtrate was taken for analysis. An Agilent reversed phase column, Zorbax SB-C18(5 μm,4.6 mm×250 mm)was used with 0.02 mol/L ammonium acetate buffer (pH=4.8) : methanol (60∶40) as the mobile phase under the condition of isocratic elution. Diode array detection method was used for PAPB determination. Qualitative and quantitative determination of PAPB was conducted in 51 batches of commercially available cosmetics. Results:The relative standard deviations (RSD) were in the range of 1.2 %-4.4 %(n=6); the recoveries were in the range of 97.5 %-106.5 %.The method showed a good linearity within the concentration range of 5-1 000 μg/mL with correlation coefficient of 0.999 62; The detection limit was 15 mg/kg. In 51 batches of commercially available cosmetics. One batch of makeup remover showed positive resullt, which was consistent with the UV spectrum of the standard. Conclusion:We have established a HPLC method for accurate quantification of PAPB. It can be used for analyzing the cosmetics products.

17.
Article in Chinese | WPRIM | ID: wpr-888141

ABSTRACT

In view of the current inadequate standards for Gleditsiae Spina in the Chinese Pharmacopoeia, this study put forward some new items of the quality standards of Gleditsiae Spina. Thin-layer chromatography(TLC) was performed for identification with the reference substance of taxifolin and the reference material of Gleditsiae Spina as the control. According to the general principles of the Chinese Pharmacopoeia(2020 edition, Vol. 4), the moisture, total ash content, and alcohol-soluble extract of medicinal materials and decoction pieces of Gleditsiae Spina were determined. The content determination method for medicinal materials and decoction pieces of Gleditsiae Spina was established using high-performance liquid chromatography(HPLC), with taxifolin as the quality control index. Based on the determination results of 30 batches of samples of Gleditsiae Spina from different habitats, the draft quality standards of Gleditsiae Spina were developed, which provided suggestions for the revision of the quality standards of Gleditsiae Spina in the Chinese Pharmacopoeia.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Quality Control , Reference Standards
18.
Int J Pharm Pharm Sci ; 2020 Apr; 12(4): 12-15
Article | IMSEAR | ID: sea-206073

ABSTRACT

Objective: The present study deals with the development, validation and application of a simple, precise and accurate HPLC method for the determination of mycophenolate mofetil in pharmaceutical formulations and microemulsions. Methods: In this method, a simple isocratic mobile phase composition of methanol and water (75:25 v/v) pumped at 1 ml/minute flow rate through Phenomenex C18 column (dimension: 250 4.6 mm and 5 µm particle size) was used. Injection volume was 20 µl and analysis of mycophenolate mofetil was carried out at 250 nm. Results: The coefficient of regression was found to be 0.9996, indicating the linearity of the developed method within a range of 0.1 to 10 µg/ml. The limit of detection (LOD) and the limit of quantization (LOQ) were found to be 3.660ng/ml and 11.091ng/ml, respectively. The results showed that % deviation for change in compositions of the mobile phase, flow rate and temperature was within a range of-5.51 to 10.99%,-3.70 to 8.80% and-5.29 to 10.90%, respectively. The method seemed sensitive to change of temperature (±5 ○C) and methanol composition (±2%) as the results were at the boundary limit of 10% deviation. Conclusion: A simple, precise and accurate HPLC method for the determination of drug content from microemulsion has been developed and validated in accordance with ICH guidelines.

19.
Article in Chinese | WPRIM | ID: wpr-845172

ABSTRACT

Objective: To provide a scientific basis for the quality control of YuanZhi San capsule(YZSC). Methods: Fourier transform infrared spectroscopy(FTIR)combined with second derivative spectra was used to analyze the chemical components of YZSC;high performance liquid chromatography(HPLC)was used to establish the fingerprints of different batches of YZSC, the quality assessment of YZSC was carried out by similarity evaluation, cluster analysis(CA), principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA). Results: The main components of YZSC were carbohydrate, flavonoids, alkaloids, organic acids and saponins. There were 41 common peaks in the fingerprint, seven peaks were identified using reference substance, they were 3, 6'-disinapoylsucrose, ferulic acid, jatrorrhizine hydrochloride, palmatine chloride, berberine, quercetin and β-asarone. The similarity of 10 batches of samples was higher than 0.99. The CA and PCA analysis indicated that there were differences in different batches of YZSC, and they were mainly divided into two categories. By the OPLS-DA, 10 main chemical constituents were found to be the cause of the quality differences in the batches, and the peaks of berberine, 3, 6'-disinapoylsucrose, palmatine chloride, β-asarone, and jatrorrhizine hydrochloride were recognized by comparison with the reference substances. Conclusion: The chemical pattern recognition technology based on the FTIR and HPLC analysis might be used for the quality evaluation of YZSC.

20.
Article in Chinese | WPRIM | ID: wpr-845155

ABSTRACT

In recent years, charged aerosol detector(CAD)has become a valuable tool for detecting substances with no ultraviolet absorption or with only end absorption. Its advantages inclucle broad linearity response range, high sensitivity and reproducibility, the signal response consistency independent of chemical structures, as well as the simply operable feature. This article briefly describes the working principle of CAD and introduces the application progress of the detector in the natural product and pharmaceutical detection as well as in the sugar, lipid, amino acid and surfactant analysis, so as to provide a reference for the liquid chromatographic analysis of non-volatile and semi-volatile compounds.

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