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1.
Journal of Pharmaceutical Practice ; (6): 78-81, 2024.
Artigo em Chinês | WPRIM | ID: wpr-1006845

RESUMO

Objective To establish method for simultaneous determination of hesperidin, cinnamaldehyde and eugenol in Chunyang Zhengqi capsules by high performance liquid chromatography. Methods The column was Agilent PorosheⅡ 120 EC-C18 (4.6 mm×150 mm, 4 μm). The mobile phase was acetonitrile-water with gradient elution. The column temperature was 35℃. The flow rate was 1.0 ml/min, and the detection wavelength was 284 nm. Results The methodological verification showed that hesperidin, cinnamaldehyde and eugenol had a good linearity (r≥0.999 9). The precisions were less than 2.0%. The average recovery was between 98.0% and 101.9%. The stability and repeatability of RSD were also less than 3.0%, which met the requirements of method validation. Conclusion The method is simple, stable, reproducible and accurate, which could be used to the quality control of Chunyang Zhengqi capsules.

2.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 143-151, 2024.
Artigo em Chinês | WPRIM | ID: wpr-1006279

RESUMO

ObjectiveTaking Achyranthis Bidentatae Radix(ABR) from different origins as samples, to quantitatively analyze the chemical composition and chromaticity of ABR with different processing degrees, and clarify the correlation and change law between color and composition in the processing process of ABR, so as to provide reference for the quality evaluation of processed products of ABR. MethodThe colorimeter is used to measure the chromaticity values of three kinds of processing degrees of ABR in different origins to show the color value change trend during the processing process, and the color parameters of wine-processed and salt-processed products of ABR with different processing degrees were analyzed by principal component analysis(PCA), orthogonal partial least squares-discriminant analysis(OPLS-DA) and other analysis methods. The contents of eight representative components of ABR were measured by high performance liquid chromatography(HPLC), the correlation between chromaticity and each representative component was analyzed by Pearson correlation analysis, and the applicability of the selected eight representative components was further verified by Fisher linear discriminant analysis, and the wine-processed and salt-processed products of ABR with different processing degrees were grouped according to the degree of processing, and 48 samples of wine-processed and salt-processed products with different processing degrees were used as training samples. Taking the contents of 5-hydroxymethylfurfural, polypodine B, β-ecdysterone, 25R-inokosterone, 25S-inokosterone, ginsenoside Ro, chikusetsusaponin Ⅳa and polysaccharides as variables, the discriminant function was established respectively, and 12 samples of wine-processed and salt-processed products of ABR with different processing degrees were back-tested to verify the discriminant function and test the reliability of the function. ResultPCA and OPLS-DA results showed that ABR samples with different processing degrees were classified into clusters, and the results could significantly distinguish different processed products. During the process of wine and salt processing, the contents of 5-hydroxymethylfurfural, ginsenoside Ro, and chikusetsusaponin Ⅳa gradually increased with the deepening of the processing degree, while the contents of polypodine B, β-ecdysterone, 25R-inokosterone, 25S-inokosterone and polysaccharides showed a gradual decreasing trend, indicating these 8 components increased and decreased to different degrees in the process of wine and salt processing. The results of Pearson correlation analysis showed that the 5-hydroxymethylfurfural content of the samples with different processing degrees of wine-processed and salt-processed products were negatively correlated with the brightness value(L*) and the total color difference value(E*ab)(P<0.01), and positively correlated with the red-green value(a*) and the yellow-blue value(b*)(P<0.01), and that the content of polypodine B and polysaccharides were positively correlated with L* and E*ab(P<0.01). The discriminant functions of wine-processed and salt-processed products of ABR were established by Fisher linear discriminant analysis, and their accuracy rates in the training samples were 93.75% and 95.83%, respectively. Twelve test samples of wine-processed and salt-processed products with different processing degree were back substitution, and the correct rate was 100%. ConclusionThe trend of composition and color changes of ABR with different processing degrees in different production areas is relatively consistent, and the color value can better distinguish ABR with different processing degrees, and the color of ABR is related to some representative components in the processing process, indicating that the color can provide reference for the identification of the processing degree of ABR and the prediction of component content.

3.
China Pharmacy ; (12): 948-954, 2024.
Artigo em Chinês | WPRIM | ID: wpr-1016717

RESUMO

OBJECTIVE To establish a method for the content determination of 11 components such as protodioscin in Guge fengtong tablets, and to evaluate the comprehensive quality of Guge fengtong tablets by combining with chemometric analysis and entropy weight-technique for order preference by similarity to ideal solution (EW-TOPSIS) method. METHODS HPLC method was adopted. The determination was performed on Agilent Eclipse Plus C18 column with a mobile phase consisted of acetonitrile- 0.2% phosphoric acid solution at the flow rate of 1.0 mL/min by gradient elution. The column temperature was set at 30 ℃ . The detection wavelengths were set at 203 nm (0-28 min, protodioscin, methyl protodioscin, pseudoprotodioscin, dioscin) and 280 nm (28-60 min, catechin, epicatechin, liquiritigenin, medicarpin, 6-gingerol, 8-gingerol, 10-gingerol); the sample size was 10 μL. Using epicatechin as the internal reference, quantitative analysis of multi-components by single marker (QAMS) method was used to determine the contents of protodioscin, methyl protodioscin, pseudoprotodioscin, dioscin, catechin, liquiritigenin, medicarpin, 6-gingerol, 8-gingerol and 10-gingerol, which were compared with the results of the external standard method. SPSS 26.0 software and SIMCA 14.1 software were used for principal component analysis and orthogonal partial least squares-discriminant analysis, with variable importance in projection (VIP) value greater than 1 as the standard, to screen for differential markers that affect the quality; the EW-TOPSIS method was adopted to evaluate the quality of 15 batches of samples comprehensively.RESULTS The contents of protodioscin, methyl protodioscin, pseudoprotodioscin, dioscin, catechin, liquiritigenin, medi-carpin, 6-gingerol, 8-gingerol and 10-gingerol determined by HPLC combined with QAMS were 6.330-10.863, 1.150-2.274, 0.431- 0.740, 2.818-4.823, 0.826-1.510, 0.043-0.094, 0.079-0.231, 0.479-1.020, 0.146-0.288, 0.118-0.318 mg/g, respectively; there were no statistical significances, compared with the external standard method (P>0.05). A total of 15 batches of samples were clustered into 3 groups, with S1-S6, S7-S10, and S11-S15 clustered into one group, respectively. The VIP values of protodioscin, epicatechin, dioscin and 6-gingerol were greater than 1. Euclidean closeness values of the optimal solution (C)i for 15 batches of samples were 0.163 5 to 0.703 7, and Ci values of S11-S15 were all higher than 0.6. CONCLUSIONS The established QAMS method is accurate and simple, and can be used for comprehensive quality evaluation of Guge fengtong tablets, by combining with chemometric analysis and EW-TOPSIS method. Protodioscin, epicatechin, dioscin and 6-gingerol are the differential markers that affect the quality of Guge fengtong tablets. Samples S11-S15 have better quality.

4.
China Pharmacy ; (12): 801-806, 2024.
Artigo em Chinês | WPRIM | ID: wpr-1013540

RESUMO

OBJECTIVE To establish an HPLC fingerprint of Xiao’er resuqing oral liquid, and to determine the contents of twelve index components. METHODS HPLC method was adopted. The determination was performed on Venusil MP C18 column with mobile phase consisting of acetonitrile-0.1% phosphate aqueous solution (gradient elution) at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm, the column temperature was 30 ℃, the injection volume was 10 μL. HPLC fingerprint of Xiao’er resuqing oral liquid was established by using the Similarity Evaluation System of Chromatographic Fingerprint of TCM (2012 edition) to evaluate the similarity. The contents of 12 components were determined, including (R, S)-goitrin, 3,5-O-dicaffeoyl quinic acid, puerarin, forsythin, forsythoside A, chlorogenic acid, baicalin, saikosaponins d, wogonoside, baicalein, emodin and chrysophanol. RESULTS The similarity of HPLC fingerprints of 13 batches of Xiao’er resuqing oral liquid was greater than 0.97, and 14 common peaks were confirmed. The contents of the above 12 index components in 13 batches of Xiao’er resuqing oral liquid were as follows: 0.078-0.172, 1.564-2.736, 1.338-2.578, 0.426-0.872, 1.477-2.628, 1.396-2.447, 4.052-9.146, 0.367- 0.692, 1.974-4.674, 1.274-2.969, 0.085-0.167 and 0.155-0.307 mg/mL. CONCLUSIONS The established HPLC fingerprint and content determination methods have high accuracy and high specificity, which can be used for the quality evaluation of Xiao’er resuqing oral liquid.

5.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 125-131, 2024.
Artigo em Chinês | WPRIM | ID: wpr-1013368

RESUMO

ObjectiveTo improve the quality standard of Yuanhu Zhitong oral liquid in order to strengthen the quality control of this oral liquid. MethodThin layer chromatography(TLC) was used for the qualitative identification of Corydalis Rhizoma and Angelicae Dahuricae Radix in Yuanhu Zhitong oral liquid by taking tetrahydropalmatine, corydaline reference substances and Corydalis Rhizoma reference medicinal materials as reference, and cyclohexane-trichloromethane-methanol(5∶3∶0.5) as developing solvent, Corydalis Rhizoma was identified using GF254 glass thin layer plate under ultraviolet light(365 nm). And taking petroleum ether(60-90 ℃) -ether-formic acid(10∶10∶1) as developing solvent, Angelicae Dahuricae Radix was identified using a silica gel G TLC plate under ultraviolet light(305 nm). High performance liquid chromatography(HPLC) was performed on a Waters XSelect HSS T3 column(4.6 mm×250 mm, 5 μm) with acetonitrile(A)-0.1% glacial acetic acid solution(adjusted pH to 6.1 by triethylamine)(B) as the mobile phase for gradient elution(0-10 min, 20%-30%A; 10-25 min, 30%-40%A; 25-40 min, 40%-50%A; 40-60 min, 50%-60%A), the detection wavelength was set at 280 nm, then the fingerprint of Yuanhu Zhitong oral liquid was established, and the contents of tetrahydropalmatine and corydaline were determined. ResultIn the thin layer chromatograms, the corresponding spots of Yuanhu Zhitong oral liquid, the reference substances and reference medicinal materials were clear, with good separation and strong specificity. A total of 12 common peaks were identified in 10 batches of Yuanhu Zhitong oral liquid samples, and the peaks of berberine hydrochloride, dehydrocorydaline, glaucine, tetrahydropalmatine and corydaline. The similarities between the 10 batches of samples and the control fingerprint were all >0.90. The results of determination showed that the concentrations of corydaline and tetrahydropalmatine had good linearity with paek area in the range of 0.038 6-0.193 0, 0.034 0-0.170 0 g·L-1, respectively. The methodological investigation was qualified, and the contents of corydaline and tetrahydropalmatine in 10 batches of Yuanhu Zhitong oral liquid samples were 0.077 5-0.142 9、0.126 1-0.178 2 g·L-1, respectively. ConclusionThe established TLC, fingerprint and determination are simple, specific and reproducible, which can be used to improve the quality control standard of Yuanhu Zhitong oral liquid.

6.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 161-166, 2023.
Artigo em Chinês | WPRIM | ID: wpr-953936

RESUMO

ObjectiveTo clone coumarate-3-hydroxylase gene (C3H) from Angelica sinensis, and analyze the correlation between its bioinformatics, expression patterns and content of ferulic acid, and to explore the functions of ASC3H. MethodReal-time polymerase chain reaction (Real-time PCR) was used to clone the full-length cDNA of ASC3H based on the transcriptome dataset of A. sinensis, and the bioinformatics analysis of the gene sequence was carried out. Real-time PCR and high performance liquid chromatography (HPLC) were used to determine relative expression of ASC3H and content of ferulic acid in different root tissues of A. sinensis (periderm, cortex and stele). ResultThe open reading frame (ORF) of ASC3H (GenBank accession number: MN2550298) was 1 530 bp, encoding 509 amino acids, with a theoretical molecular weight of 57.86 kDa and an isoelectric point of 8.36. It was a hydrophilic protein that was located in the chloroplast with multiple phosphorylation sites and a transmembrane region, and contained a conserved domain CGYDWPKGYGPIINVW_P450 (383-399 aa) in cytochrome P450. Multiple amino acid sequence alignment analysis showed that ASC3H had high similarity with C3H from other plants, especially Ammi majus in Umbelliferae. The Real-time PCR revealed that ASC3H had different expressions in periderm, cortex and stele tissues of A. sinensis roots. It was found from HPLC that the cortex tissues had the highest content of ferulic acid, and the stele tissues had the lowest. ConclusionASC3H was successfully cloned from A. sinensis, and its sequence characteristics were understood more clearly, suggesting that ASC3H might be involved in the ferulic acid biosynthesis pathway of A. sinensis. This paper provided a basis for further studying the functions of the gene and exploring the biosynthesis and regulation mechanism of ferulic acid in A. sinensis, while laying the foundation for the genetic improvement of A. sinensis.

7.
Journal of China Pharmaceutical University ; (6): 749-756, 2023.
Artigo em Chinês | WPRIM | ID: wpr-1003595

RESUMO

@#The UPLC fingerprint of colistimethate sodium was established for the study of quality consistency.The chromatographic column was Acquity UPLC? Peptide CSH C18 (2.1 mm × 150 mm, 1.7 μm).The mobile phase A was phosphate buffer-acetonitrile (19∶1), and the mobile phase B was phosphate buffer-acetonitrile (1∶1).The mobile phase was in gradient elution at a flow rate of 0.3 mL/min.The column temperature was set at 30 °C and the detection wavelength was 210 nm.The similarity of the fingerprints was analyzed with the Similarity Evaluation System for Chromatographic Fingerprint of Tradition Chinese Medicine (Version 2012) in combination with content determination of multiple index components to evaluate the quality consistency of imported and domestic bulk drugs.The result showed that both the original and generic bulk drugs met the specified limit requirements in the European Pharmacopoeia standards, and that their UPLC fingerprints were highly similar, indicating that the quality of the two substances was consistent.Establishing a fingerprint for similarity evaluation and combining it with the results of indicator component content determination as a comprehensive evaluation method for the study of drug quality consistency of complex components has the characteristics of fast, accurate, and comprehensive, which is helpful for drug quality evaluation and provides ideas for the evaluation of antibiotic quality consistency of complex components.

8.
China Pharmacy ; (12): 802-806, 2023.
Artigo em Chinês | WPRIM | ID: wpr-969575

RESUMO

OBJECTIVE To establish comprehensive quality evaluation method based on multi-index components combined with multivariate statistical analysis, and to comprehensively evaluate the quality of Periploca forrestii. METHODS Taking 11 batches of P. forrestii medicinal materials from different areas in Guizhou as samples, the contents of neochlorogenic acid, cryptochlorogenic acid, chlorogenic acid, procyanidin A2, isochlorogenic acid A and isochlorogenic acid C were determined by HPLC. Clustering heat map analysis, grey correlation analysis(GRA) and technique for order preference by similarity to ideal solution(TOPSIS) were used to evaluate the quality of P. forrestii. RESULTS The results of methodological investigation of content determination were in accordance with the relevant regulations, and the linear relationship and accuracy of each component were good in their respective sampling range. The contents of chlorogenic acid, cryptochlorogenic acid, neochlorogenic acid, procyanidin A2, isochlorogenic acid A and isochlorogenic acid C in 11 batches of samples were 3.650-7.302, 0.888-2.575, 1.371- 2.386, 0.947-1.469, 0.084-0.169 and 0.725-1.067 mg/g, respectively. The content of each component was significantly different, with the highest content of chlorogenic acid and the lowest content of isochlorogenic acid A. The comprehensive results of cluster heat map, GRA and TOPSIS analysis showed that the comprehensive quality of S5 and S10 was relatively good. CONCLUSIONS The established method is accurate, stable and simple. Combined with multivariate statistical analysis method, it can be used for quality evaluation of P. forrestii. The quality of samples from Jiuzhou Town and Caiguan Town of Xixiu District in Anshun City of Guizhou Province are relatively good among 11 different origin samples.

9.
Journal of Pharmaceutical Practice ; (6): 192-196, 2023.
Artigo em Chinês | WPRIM | ID: wpr-965572

RESUMO

Objective To establish a method for the determination of cisatracurium besylate in human plasma by UPLC-MS/MS which could be used in the monitoring of drug residual in plasma of elderly patients after operation. Methods The samples were precipitated with 0.1% formic acid-acetonitrile solution and separated by an SHISEIDO ADME column(3.0 mm×100 mm, 2.7 μm) for isocratic elution with the mobile phase of water containing 0.1% formic acid with 2 mmol/L ammonium acetate and acetonitrile (30:70, V/V). MS condition was optimized in the positive ion detection mode by multiple reaction monitoring (MRM), along with the Agilent jet stream electrospray source interface (AJS-ESI). The precursors to the product ion transitions were m/z 464.3→358.2 for cisatracurium besylate and m/z 557.4→356.3 for vecuronium bromide (the internal standard, IS). Plasma samples of elderly patients undergoing spinal surgery were collected after anesthesia induction, at the end of surgery, 0.5 h and 1 h after surgery, and from the blood bags while autologous blood transfusion, and stored in cryopreservation tubes with 2% formic acid solution. Then the contents of cisatracurium besylate were determined. The effects of autogenous blood transfusion on plasma concentration of cisatracurium besylate in elderly patients after surgery evaluated. Results The calibration curve was linear in the range of 20-5 000 ng/ml for cisatracurium besylate in human plasma, r=0.999 7. The intra-day and inter-day precision and accuracy were good (RSD<10%, RE<±10%). The matrix effect of different concentrations was 71.88%~80.64%. The recovery of different concentrations was 83.62%~88.87%. The recovery of vecuronium bromide (IS) was 125.91%, which conformed with the requirement of methodological validation. There was a certain degree of residual cisatracurium besylate in the plasma of elderly patients, so the extubation time should be strictly controlled and the stay time of patients in the anesthesia recovery room should be appropriately extended. Conclusion The method is sensitive, accurate, and efficient, which could be used for the determination of cisatracurium besylate in human plasma of elderly patients after operation.

10.
China Pharmacy ; (12): 682-686, 2023.
Artigo em Chinês | WPRIM | ID: wpr-965505

RESUMO

OBJECTIVE To establish the quality standard of Clinopodium gracile. METHODS Ten batches of C. gracile were collected to perform appearance and property identification, microscopic identification and thin layer chromatography (TLC) identification. Moisture, total ash, acid-insoluble ash and dilute ethanol extract were detected, and the content of rosmarinic acid was determined by HPLC. RESULTS The stem of C. gracile was slender, square columnar, covered by white fluff, the surface was grayish green or greenish brown; epidermal cells, non-glandular hairs, cortical cells and so on were seen in the cross section of the stem. Non-glandular hairs, ducts, wood fibers, mesophyll cells and so on could be seen in the powder. Results of TLC identification showed that there were spots of the same color in the chromatographic position corresponding to the chromatographic position of buddlejasaponin Ⅳb control. The contents of water, total ash, acid-insoluble ash, dilute ethanol extract and rosmarinic acid in 10 batches of samples were 8.69%-12.33%, 5.96%-13.33%, 0.14%-3.29%, 18.57%-32.61%, 0.35%-0.82%, respectively. The average values were 10.10%, 9.73%, 1.06%, 23.54% and 0.56%, respectively. CONCLUSIONS The established method can be used for quality control of C. gracile. It is preliminarily proposed that the ash content in the herb should not exceed 12.0%, the total ash content should not exceed 12.0%, the acid-insoluble ash content should not exceed 1.5%, the dilute ethanol extract should not be less than 18.0%, and the rosmarinic acid content should not be less than 0.45%.

11.
Acta Pharmaceutica Sinica ; (12): 201-207, 2023.
Artigo em Chinês | WPRIM | ID: wpr-964309

RESUMO

Based on ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), a rapid and simultaneous quantitative method for the measurement of seven components (kinsenoside; rutin; kaempferol-3-O-rutinoside; quercimeritrin; narcissin; isorhamnetin-3-O-glucoside; quercetin) of A. roxburghii was established. The separation was performed over 8.0 minutes on a Waters Acquity UPLC BEH Shield RP18 (2.1 mm × 100 mm; 1.7 μm) with a mobile phase consisting of acetonitrile (A) and 0.1% formic acid water solution (B) with gradient elution at a flow rate of 0.2 mL·min-1; the column temperature was 30 ℃ and the injection volume was 2 μL. Electrospray spray ionization source (ESI source) was used for mass spectrometry, and positive and negative ion modes were detected at the same time. The results showed good linearity (R2 ≥ 0.998 0), with good precision, repeatability and stability, and the average recovery was 97.71%-103.33%. Through cluster heat map and redundancy analysis, we found that kinsenoside was mainly distributed in stems, followed by leaves, and the lowest content in roots. The content of kinsenoside increased significantly in the stems of plants 6 months, but less change was evident in the roots and leaves. Flavonoids and flavonoid glycosides were mainly distributed in leaves. The UHPLC-MS/MS method established in this paper can be used for the quality control of A. roxburghii and provides a reference for establishing a more comprehensive quality detection method for this medicinal.

12.
Journal of Pharmaceutical Practice ; (6): 119-124, 2023.
Artigo em Chinês | WPRIM | ID: wpr-964284

RESUMO

Objective To optimize the microwave-assisted extraction process of green tea polyphenols. Methods The extraction yield of tea polyphenols was figured up by building the standard curve of gallic acid and examining the concentration of tea polyphenols in green tea extract with the introduction of a correction factor. The effects of four single factor levels of microwave extraction time, microwave output power, liquid-to-material yield, and ethanol volume fraction on the extraction yield of tea polyphenols were primarily studied in this experiment. The response surface was applied to further optimize the extraction process of green tea polyphenols after exploring the appropriate range of four single factor levels. Results The optimal extraction process was as follows: extraction time 37 s, microwave output power 350 w, material - liquid yield 1∶45 (g/ml), ethanol volume fraction 55%, and the actual extraction yield of tea polyphenols was 25.65%, which was not much different from the theoretical value. Conclusion The microwave-assisted green tea polyphenol extraction process optimized by response surface methodology is time-saving and practicable, and the extraction yield is high.

13.
China Journal of Chinese Materia Medica ; (24): 3806-3814, 2023.
Artigo em Chinês | WPRIM | ID: wpr-981513

RESUMO

The weight coefficients of appearance traits, extract yield of standard decoction, and total content of honokiol and magnolol were determined by analytic hierarchy process(AHP), criteria importance though intercrieria correlation(CRITIC), and AHP-CRITIC weighting method, and the comprehensive scores were calculated. The effects of ginger juice dosage, moistening time, proces-sing temperature, and processing time on the quality of Magnoliae Officinalis Cortex(MOC) were investigated, and Box-Behnken design was employed to optimize the process parameters. To reveal the processing mechanism, MOC, ginger juice-processed Magnoliae Officinalis Cortex(GMOC), and water-processed Magnoliae Officinalis Cortex(WMOC) were compared. The results showed that the weight coefficients of the appearance traits, extract yield of standard decoction, and total content of honokiol and magnolol determined by AHP-CRITIC weighting method were 0.134, 0.287, and 0.579, respectively. The optimal processing parameters of GMOC were ginger juice dosage of 8%, moistening time of 120 min, and processing at 100 ℃ for 7 min. The content of syringoside and magnolflorine in MOC decreased after processing, and the content of honokiol and magnolol followed the trend of GMOC>MOC>WMOC, which suggested that the change in clinical efficacy of MOC after processing was associated with the changes of chemical composition. The optimized processing technology is stable and feasible and provides references for the modern production and processing of MOC.


Assuntos
Zingiber officinale , Magnolia/química , Medicamentos de Ervas Chinesas/química , Compostos de Bifenilo/química , Lignanas/química
14.
China Journal of Chinese Materia Medica ; (24): 3516-3534, 2023.
Artigo em Chinês | WPRIM | ID: wpr-981484

RESUMO

Ultra-high performance liquid chromatography-quadrupole-Exactive Orbitrap high resolution mass spectrometry(UHPLC-Q-Exactive Orbitrap HRMS) was employed to systematically analyze the chemical constituents in Lysionoti Herba, and high perfor-mance liquid chromatography-ultraviolet(HPLC-UV) to determine the content of main compounds. A Synergi~(TM) Hydro-RP 100 Å colu-mn(2 mm×100 mm, 2.5 μm) was used for gradient elution with acetonitrile-0.1% aqueous formic acid as the mobile phase at a flow rate of 0.2 mL·min~(-1) and a column temperature of 40 ℃. MS and MS/MS were conducted with electrospray ionization(ESI) in both positive and negative modes. The chemical components in Lysionoti Herba were identified by comparison with the retention time and mass spectra of reference compounds and the relevant mass spectral data reported in MS databases and relevant literature. Furthermore, the content of five constituents(neochlorogenic acid, chlorogenic acid, forsythoside B, acteoside, and nevadensin) in different Lysiono-ti Herba samples was simultaneously determined by HPLC-UV at the wavelength of 330 nm. A total of 84 compounds were identified in Lysionoti Herba, including 27 flavonoids, 20 phenylethanoid glycosides, 5 amino acids, 18 organic acids, 1 alkaloid, 6 nucleosides, and 7 others. The content of neochlorogenic acid, chlorogenic acid, forsythoside B, acteoside, and nevadensin showed good linear relationship(r>0.999) with the peak area within certain concentration ranges, which were 3.22-102.90, 12.84-410.82, 31.63-1 012.01, 25.00-800.11, and 4.08-130.51 μg·mL~(-1), respectively. The instrument precision, method repeatability, and solution stability all met requirement, and the average recovery rate was 97.31%-100.2%, with RSD ranging from 0.95% to 2.4%. The content of the five components varied among different Lysionoti Herba samples collected from different regions of Guizhou, and the average content of forsythoside B was the highest. The established qualitative method can rapidly and efficiently identify the chemical components of Lysionoti Herba, and the developed HPLC-UV method can simultaneously determine the content of five components in a simple, ra-pid, and accurate manner, providing a scientific basis for the quality evaluation of Lysionoti Herba.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas em Tandem/métodos , Ácido Clorogênico , Medicamentos de Ervas Chinesas/química
15.
China Journal of Chinese Materia Medica ; (24): 3000-3013, 2023.
Artigo em Chinês | WPRIM | ID: wpr-981446

RESUMO

Huocao(a traditional Chinese herbal medicine) moxibustion is a characteristic technology in Yi medicine suitable for cold-dampness diseases. Huocao, as the moxibustion material, is confusedly used in clinical practice and little is known about its quality control. In this study, UPLC method was used to establish the chemical fingerprint of non-volatile components in Huocao, and the contents of eight phenolic acids such as chlorogenic acid were determined. Multivariate statistical analysis was performed to obtain the indicator components of Huocao for quality evaluation, and thus a comprehensive evaluation system for the quality of Huocao was built. The UPLC fingerprints of 49 batches of Huocao were established, and there were 20 common peaks, of which eight phenolic acids including neochlorogenic acid and chlorogenic acid were identified. Except for three batches of Huocao, the similarity of the other 46 batches was higher than 0.89, suggesting that the established fingerprint method could be used for quality control of the medicinal herb. The correlation coefficient between entropy weight score of the eight phenolic acids and comprehensive fingerprint score in Huocao was 0.875(P<0.01), which indicated that the eight phenolic acids could be used as indicator components for the quality evaluation of Huocao. Furthermore, in multivariate statistical analysis on the common peaks of fingerprint and the contents of the eight phenolic acids, chlorogenic acid, isochlorogenic acid A and isochlorogenic acid C were screened to be the indicator components. The results revealed that the proposed method achieved a simple and accurate quality control of Huocao based on UPLC fingerprint and multi-component content determination, which provided useful data for establishing the quality standard of Huocao.


Assuntos
Ácido Clorogênico , Entropia , Hidroxibenzoatos , Controle de Qualidade
16.
China Journal of Chinese Materia Medica ; (24): 2781-2791, 2023.
Artigo em Chinês | WPRIM | ID: wpr-981381

RESUMO

Rosae Radix et Rhizoma is a herbal medicine in a variety of famous Chinese patent medicines, while the quality standard for this medicine remains to be developed due to the insufficient research on the quality of Rosae Radix et Rhizoma from different sources. Therefore, this study comprehensively analyzed the components in Rosae Radix et Rhizoma of different sources from the aspects of extract, component category content, identification based on thin-lay chromatography, active component content determination, and fingerprint, so as to improve the quality control. The results showed that the content of chemical components varied in the samples of different sources, while there was little difference in the chemical composition among the samples. The content of components in the roots of Rosa laevigata was higher than that in the other two species, and the content of components in the roots was higher than that in the stems. The fingerprints of triterpenoids and non-triterpenoids were established, and the content of five main triterpenoids including multiflorin, rosamultin, myrianthic acid, rosolic acid, and tormentic acid in Rosae Radix et Rhizoma was determined. The results were consistent with those of major component categories. In conclusion, the quality of Rosae Radix et Rhizoma is associated with the plant species, producing area, and medicinal parts. The method established in this study lays a foundation for improving the quality standard of Rosae Radix et Rhizoma and provides data support for the rational use of the stem.


Assuntos
Medicamentos de Ervas Chinesas/química , Rizoma/química , Raízes de Plantas/química , Plantas Medicinais , Controle de Qualidade
17.
China Journal of Chinese Materia Medica ; (24): 2086-2091, 2023.
Artigo em Chinês | WPRIM | ID: wpr-981340

RESUMO

We explored the correlations between the color difference values [ΔL~*(lightness), Δa~*(red-green), Δb~*(yellow-blue)] and the content of four active components(including sesquiterpenoids and polyacetylenes) in the powder of Atractylodes lancea and A. chinensis, aiming to provide reference for the quality evaluation of Atractylodis Rhizoma and establish a qualitative model that can distinguish between A. lancea and A. chinensis based on the chromatic values. The tristimulus values(L~*, a~*, and b~*) of 23 batches of A. lancea and A. chinensis were measured by a color difference meter. The content of atractylenolide Ⅱ, β-eudesmol, atractylodin, and atractylone in the 23 batches of samples were measured by high performance liquid chromatography(HPLC). Principal component analysis(PCA) and partial least squares-discriminant analysis(PLS-DA) were performed to establish the qualitative models for distinguishing between A. lancea and A. chinensis. SPSS was employed to analyze the correlations between the tristimulus values and the content of the four index components. The results showed that the established PCA and PLS-DA models can divide the A. lancea and A. chinensis samples into two regions, and the tristimulus values of A. lancea and A. chinensis were positively correlated with the content of β-eudesmol and atractylodin. Therefore, the PCA and PLS-DA models can successfully identify A. lancea and A. chinensis, and the appearance color can be used to quickly predict the internal quality of Atractylodis Rhizoma. This study provides a reference for the quality evaluation of Atractylodis Rhizoma and the modern research on the color of Chinese medicinal materials.


Assuntos
Atractylodes , Sesquiterpenos de Eudesmano , Medicamentos de Ervas Chinesas , Rizoma , Excipientes
18.
China Journal of Chinese Materia Medica ; (24): 2435-2454, 2023.
Artigo em Chinês | WPRIM | ID: wpr-981320

RESUMO

This study aimed to investigate the impact of ginger juice on chemical profile of Magnoliae Officinalis Cortex(MOC) when they were processed together. Ultra-high-performance liquid chromatography coupled to quadrupole-orbitrap high-resolution mass spectrometry(UHPLC-Q-Orbitrap HRMS) was used for qualitative analysis of the chemical component of MOC samples before and after being processed with ginger juice. UPLC was performed to observe the content variation of eight main components in processed MOC. A total of 174 compounds were identified or tentatively deduced from processed and unprocessed MOC samples according to MS data obtained in positive and negative ion mode. After MOC was processed with ginger juice, the peak areas of most phenolics increased, while the peak areas of most phenylethanoid glycosides decreased; as for neolignans, oxyneolignans, other lignans and alkaloids, changes in the peak area were variable, and the peak areas of terpenoid-lignans varied little. Additionally, gingerols and diarylheptanoids were only detected in the processed MOC sample. The contents of syringin, magnoloside A, and magnoloside B decreased significantly in the processed MOC sample while no significant difference was observed in the contents of magnoflorine, magnocurarine, honokiol, obovatol, and magnolol. This study comprehensively explored the content variation of chemical components in processed and unprocessed MOC samples derived from different regions and with different tree ages using UPLC and UHPLC-Q-Orbitrap HRMS, and summarized the variation characteristics of various compounds. The results provide a data foundation for further research on pharmacodynamic substances of MOC processed with ginger juice.


Assuntos
Zingiber officinale , Árvores , Cromatografia Líquida de Alta Pressão/métodos , Alcaloides , Lignanas/análise
19.
China Pharmacy ; (12): 1949-1954, 2023.
Artigo em Chinês | WPRIM | ID: wpr-980586

RESUMO

OBJECTIVE To establish the fingerprints of Ardisia crenata, Sophora tonkinensis and their couplet medicines, and to determine the contents of five components in them. METHODS Using water as solvent, single lyophilized powder of A. crenata and S. tonkinensis and combined lyophilized powder of their couplet medicines were prepared by combining lyophilization technology. The fingerprints of three lyophilized powder samples were established by using high-performance liquid chromatography (HPLC), and the contents of 5 kinds of components such as gallic acid were determined simultaneously. RESULTS There were 5, 10 and 14 common peaks in the fingerprints for single lyophilized powder of A. crenata and S. tonkinensis and combined lyophilized powder of their couplet medicines; the similarities of them with the control fingerprints were all greater than 0.90. For combined lyophilized powder of couplet medicines, peak 3 Δ 基金项目 国家重点研发计划项目(No.2018YFC1708100);贵 州省科技计划项目(No.黔科合基础-ZK〔2022〕一般483,No.黔科合成 was identified as gallic acid, peak 4 as matrine, peak 6 as 果〔2021〕一般137);贵州省教育厅高等学校科学研究项目(青年项目) oxymatrine, peak 8 as bergenin, and peak 14 as trifolirhizin. In single lyophilized powder of A. crenata, the average contents of gallic acid and bergenin were 0.499 3 and 4.962 6 mg/g, respectively. In single lyophilized powder of S.tonkinensis, the average contents of matrine, oxymatrine and trifolirhizin were 3.046 0, 2.336 6 and 0.278 6 mg/g, respectively. In combined lyophilized powder of couplet medicines, the average contents of gallic acid, matrine, oxymatrine, bergenin and trifolirhizin were 0.560 6, 2.548 7, 1.382 2, 5.960 7 and 0.279 1 mg/g, respectively. The transfer rates were 8.87%-513.19%. CONCLUSIONS The established fingerprint and content determination methods are stable and feasible, and can be used for the quality control of A. crenata and S. tonkinensis and their couplet medicines. The average contents of matrine and oxymatrine in combined lyophilized powder of A. crenata-S. tonkinensis couplet medicines are decreased.

20.
Acta Pharmaceutica Sinica ; (12): 1867-1879, 2023.
Artigo em Chinês | WPRIM | ID: wpr-978660

RESUMO

By integrating plant metabonomics and target quantitative analysis methods, this study systematically analyzed the differences of chemical constituents in Scutellaria baicalensis leaves from different producing areas in Shanxi, so as to provide theoretical basis for rational and effective utilization of Scutellaria baicalensis leaves. Based on the idea of plant metabonomics, the liquid quality of 53 batches of Scutellaria baicalensis leaves from 8 different producing areas in Shanxi was analyzed by UPLC-QTOF-MS, and the collected data were imported into SIMCA 14.1 software for multivariate statistical analysis to screen the different chemical constituents among different habitats in Shanxi. Meanwhile, a method for simultaneous determination of 7 flavonoids and 3 organic acids in Scutellaria baicalensis leaves was optimized and established to quantitatively analyze the differences of chemical components in Scutellaria baicalensis leaves from different producing areas in Shanxi. The results of plant metabonomics showed that there were differences in the chemical composition of Scutellaria baicalensis leaves in northern Shanxi (Datong, Xinzhou), Jinzhong (Yangquan, Luliang) and southern Shanxi (Changzhi, Yuncheng, Jincheng, Linfen): there were 14 significant differences in chemical composition between northern Shanxi and Jinzhong; there were 18 significant differences in chemical constituents between southern Shanxi and central Shanxi. There were 15 significant differences in chemical constituents between northern Shanxi and southern Shanxi. Among them, scutellarin and isocarthamidin-7-O-glucuronide were the common differences among the three regions, and the content of scutellarin was the highest in southern Shanxi and the lowest in northern Shanxi. The content of isocarthamidin-7-O-glucuronide was the highest in Jinzhong area and the lowest in northern Shanxi area. Quantitative analysis further confirmed that the average contents of apigenin, naringenin and citric acid were the highest in northern Shanxi, scutellarin, caffeic acid, apigenin-7-O-glucuronide, malic acid and wogonoside were the highest in southern Shanxi, and wogonoside and baicalin were the highest in central Shanxi. This study is of great significance to the quality control of Scutellaria baicalensis leaf resources, and provides theoretical basis for rational and effective utilization of Scutellaria baicalensis leaf resources.

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