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1.
Journal of Pharmaceutical Practice ; (6): 78-81, 2024.
Article in Chinese | WPRIM | ID: wpr-1006845

ABSTRACT

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.
Article in Chinese | WPRIM | ID: wpr-1006279

ABSTRACT

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.
Article in Chinese | WPRIM | ID: wpr-1016717

ABSTRACT

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.
Article in Chinese | WPRIM | ID: wpr-1013540

ABSTRACT

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.
Article in Chinese | WPRIM | ID: wpr-1013368

ABSTRACT

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.
China Pharmacy ; (12): 2874-2879, 2023.
Article in Chinese | WPRIM | ID: wpr-999220

ABSTRACT

OBJECTIVE To establish the HPLC fingerprint of Jianpi huayu decoction, and to determine the contents of 8 components. METHODS Thermo Hypersil Gold C18 column was used with mobile phase consisted of methanol-0.05% phosphoric acid aqueous solution (gradient elution) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃, the injection volume was 5 μL. The detection wavelength of matrine was 211 nm, and the other components’ detection wavelength was 283 nm. The similarity evaluation of HPLC fingerprints for 10 batches of Jianpi huayu decoction was performed by using the Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine (2012 edition). The contents of chlorogenic acid, vanillic acid, p-coumaric acid, ferulic acid, hesperidin, quercetin, bergapten and matrine in the samples were determined by HPLC. RESULTS HPLC fingerprint of Jianpi huayu decoction was established. A total of 27 common peaks were identified, and 8 components were identified. The similarity between 10 batches of samples and the control map ranged from 0.942-0.999. RSDs of precision, repeatability and stability tests were less than 3% (n=6). The average recoveries of chlorogenic acid, vanillic acid, p-coumaric acid, ferulic acid, hesperidin, quercetin, bergapten and matrine were 99.48%, 101.32%, 101.18%, 100.79%, 101.12%, 99.19%, 99.81% and 102.46%, respectively; RSDs were 1.34%, 0.93%, 1.90%, 1.84%, 0.54%, 1.53%, 1.33% and 1.01%, respectively (n=6). The contents were 0.021-0.061, 0.025-0.034, 0.116-0.295, 0.006- 0.062, 0.014-0.053, 0.017-0.026, 0.014-0.027 and 14.05-24.11 mg/g, respectively. CONCLUSIONS The established fingerprint and content determination method can provide a reference for the quality control and subsequent preparation development for Jianpi huayu decoction.

7.
China Pharmacy ; (12): 2861-2867, 2023.
Article in Chinese | WPRIM | ID: wpr-999218

ABSTRACT

OBJECTIVE To establish the HPLC fingerprint of Xintongshu spray, determine the contents of identified components, and investigate the transferring patterns of the index components of decoction pieces, intermediates and spray, so as to provide scientific reference for technology management and quality control of Xintongshu spray. METHODS HPLC fingerprints of 13 batches of Xintongshu spray were established by the Similarity Evaluation System for Chromatographic Fingerprints of TCM (2012 edition), and common peaks were identified; the contents of identified components were determined by HPLC. The paeonol in Moutan Cortex and ferulic acid in Chuanxiong Rhizoma were used as index components to investigate the transferring patterns of them in decoction pieces, intermediates and spray. RESULTS There were a total of 33 common peaks in the fingerprints of 13 batches of Xintongshu spray, and the similarities were more than 0.994. Eight components were identified, i.e. gallic acid (peak 5), oxypaeoniflorin (peak 9), chlorogenic acid(peak 10), caffeic acid (peak 14), paeoniflorin (peak 17), ferulic acid (peak 21), senkyunolide Ⅰ (peak 27) and paeonol (peak 31). The contents of 8 components ranged from 0.590 3- 0.719 7, 0.565 7-0.851 3, 0.279 4-0.368 1, 0.080 6-0.106 1, 1.922 5-3.033 5, 0.151 3-0.191 6, 0.250 6-0.336 0, 3.056 7-4.161 0 mg/mL, respectively. The average transfer rates of paeonol and ferulic acid from decoction pieces to sprays were 63.76% and 38.06%, respectively. It was also found that the process in which the loss of paeonol was more than 30% was the extraction by percolation and negative pressure concentration of Moutan Cortex. The process in which the loss of ferulic acid was more than 50% was the steam distillation extraction process of Chuanxiong Rhizoma. CONCLUSIONS The established HPLC fingerprint and content determination method of Xintongshu spray are reproducible and specific. The key processes that cause a decrease in the average transfer rates of the index components are the extraction by percolation and negative pressure concentration of Moutan Cortex and steam distillation extraction of Chuanxiong Rhizoma.

8.
China Pharmacy ; (12): 2841-2847, 2023.
Article in Chinese | WPRIM | ID: wpr-999215

ABSTRACT

OBJECTIVE To optimize the extraction technology for the raw drugs of Sanse powder gel paste. METHODS SD rats were divided into blank group, model group, traditional technology group, water extraction group and ethanol extraction group, with 5 rats in each group. Anterior cruciate ligament transection was used to construct knee osteoarthritis model, and the pharmacodynamic effects of different extraction methods on arthritic rats were investigated. Analgesic experiments were conducted using cold and hot pain thresholds and pain mediators calcitonin gene-related peptide (CGRP), cyclooxygenase-2 (COX-2), substance P (SP), and prostaglandin E2 (PGE2) contents as indicators. HE staining was performed on the synovial membrane of rats to observe the degree of synovial cell proliferation, inflammatory infiltration and vascular invasion, and anti-inflammatory experiments were conducted using protein and mRNA expressions of interleukin-1β (IL-1β), tumor necrosis factor-α (TNF-α) and IL-6 as indicators. The analgesic and anti-inflammatory effects were compared among those groups. In the orthogonal test, ethanol dosage, extraction time and extraction times were used as evaluation factors, and the contents of casticin, strychnine and toxiferine were taken as evaluation indicators; comprehensive score was calculated. The validation experiments were carried out after optimizing the extraction technology of the raw drugs of Sanse powder gel paste. RESULTS Compared with the model group, the cold and heat pain thresholds of drug administration groups (except for the traditional technology group) were all increased significantly (P<0.05), while the contents of pain (No.Y2021rc02) mediators CGRP, COX-2, SP and PGE2 were all decreased significantly (P<0.05). HE staining showed that inflammatory cell infiltration, fibrosis and collagen deposition were 炎。E-mail:liuzixiu3221@126.com decreased in the administration groups; a small amount of capillary proliferation could be found; the protein and mRNA expressions of inflammatory factors such as IL-1β, IL-6 and TNF-α were decreased significantly in synovial tissue of rats in administration groups (P<0.05). Compared with the traditional technology group, most indicators of the ethanol extraction group were significantly reduced (P<0.05), and only heat pain threshold and mRNA expression of IL-6 in rats were decreased significantly in the water extraction group (P<0.05). The optimal extraction technology of the raw drugs of Sanse powder gel paste included suitable dose of Sanse powder, 8-fold 55% ethanol, heating reflux extraction for 90 minutes, extracting twice. The results of 3 times of verification experiments showed that the average contents of casticin, strychnine and toxiferine were 0.007%, 0.092%, and 0.214%, respectively; RSD were all less than 5%. CONCLUSIONS The optimized extraction technology for the raw drugs of Sanse powder gel paste is stable and feasible, which can improve the efficacy of the preparation.

9.
China Pharmacy ; (12): 2715-2720, 2023.
Article in Chinese | WPRIM | ID: wpr-998554

ABSTRACT

OBJECTIVE To establish the fingerprint of total saponins from Mussaenda pubescens, and to study the spectrum- effect relationship of its hepatoprotective activity. METHODS Ten batches of total saponins from M. pubescens from different origins were prepared using 75% ethanol as solvent. High-performance liquid chromatography (HPLC) and the Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprints (2012 edition) were used to draw the fingerprints of 10 batches of total saponins from M. pubescens. The similarity evaluation and identification of common peaks were conducted. The same HPLC method was adopted to determine the contents of five triterpenoid saponins (mussaendoside H, mussaendoside U, mussaglaoside C, mussaendoside G and mussaendoside O). The hepatoprotective effect of total saponins from M. pubescens was investigated by establishing carbon tetrachloride-induced acute liver injury model mice, and the spectrum-effect relationship was studied by using grey correlation analysis. RESULTS There were 11 common peaks in 10 batches of total saponins from M. pubescens, 5 of which were identified, i.e. mussaendoside H (peak 3), mussaendoside U (peak 7), mussaglaoside C (peak 8), mussaendoside G (peak 9) and mussaendoside O (peak 11); the similarities of 10 batches of samples ranged 0.940- 0.991. Average contents of mussaendoside H, mussaendoside U, mussaglaoside C, mussaendoside G, mussaendoside O were 0.01- 0.05, 0.10-0.21, 0.10-0.18, 0.03-0.08, 0.20-0.40 mg/g, respectively. Ten batches of total saponins from M. pubescens could generally reduce the contents of alanine aminotransferase (ALT) and aspartate aminotransferase (AST) in serum, and tumor necrosis factor-α (TNF-α), interleukin-6 (IL-6) and IL-1β in liver tissue of model mice (P<0.05 or P<0.01). The E-mail:13878195336@139.com correlation between the common peak areas and the contents of ALT, AST, TNF-α, IL-6 and IL-1β were 0.602-0.757, 0.585-0.833, 0.593-0.795, 0.618-0.820, 0.607-0.804, respectively; the peaks with high correlation were peaks 11, 9 and 8 in order. CONCLUSIONS Ten batches of total saponins from M. pubescens have similar components, and the average contents of mussaendoside H, mussaendoside U, mussaglaoside C, mussaendoside G and mussaendoside O are different. The batches of samples have a certain degree of hepatoprotective effect; mussaendoside O, mussaendoside G and mussaglaoside C may be its main active components.

10.
China Journal of Chinese Materia Medica ; (24): 3806-3814, 2023.
Article in Chinese | WPRIM | ID: wpr-981513

ABSTRACT

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.


Subject(s)
Zingiber officinale , Magnolia/chemistry , Drugs, Chinese Herbal/chemistry , Biphenyl Compounds/chemistry , Lignans/chemistry
11.
China Journal of Chinese Materia Medica ; (24): 3516-3534, 2023.
Article in Chinese | WPRIM | ID: wpr-981484

ABSTRACT

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.


Subject(s)
Chromatography, High Pressure Liquid/methods , Tandem Mass Spectrometry/methods , Chlorogenic Acid , Drugs, Chinese Herbal/chemistry
12.
China Journal of Chinese Materia Medica ; (24): 3000-3013, 2023.
Article in Chinese | WPRIM | ID: wpr-981446

ABSTRACT

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.


Subject(s)
Chlorogenic Acid , Entropy , Hydroxybenzoates , Quality Control
13.
China Journal of Chinese Materia Medica ; (24): 2781-2791, 2023.
Article in Chinese | WPRIM | ID: wpr-981381

ABSTRACT

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.


Subject(s)
Drugs, Chinese Herbal/chemistry , Rhizome/chemistry , Plant Roots/chemistry , Plants, Medicinal , Quality Control
14.
China Pharmacy ; (12): 1354-1357, 2023.
Article in Chinese | WPRIM | ID: wpr-974684

ABSTRACT

OBJECTIVE To establish the ion mobility mass spectrometry method for simultaneous determination of epiberberine, berberine, coptisine, palmatine, calycosin-7-glucoside, 3,5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid and chlorogenic acid in Jinqi jiangtang tablets. METHODS Ion mobility mass spectrometry method was used. The determination was performed on Waters ACQUITY UPLC HSS T3 (2.1 mm×50 mm, 1.8 μm) with mobile phase consisted of 0.1% formic acid solution-acetonitrile (gradient elution) at the flow rate of 0.3 mL/min. The column temperature was 40 ℃, and the injection volume was 5 μL. The contents of 8 components in Jinqi jiangtang tablets were determined by scanning detection under positive and negative ion modes with an electric spray ion source, and setting ion mobility mass parameters according to the peak response of each component. RESULTS The results showed that the linear relationship of the eight components was good within their respective ranges (r≥0.999); RSDs of precision, repeatability and stability (24 h) tests were not more than 4.0%; average recoveries were 94.6%-101.2% , RSDs were 2.6%-3.9% (n=9). The contents of the above eight components in three batches of Jinqi jiangtang tablets were 3.060-3.545, 24.50-26.74, 2.795-4.149, 1.437-2.501, 0.204-0.242, 0.950-1.281, 2.272-2.828, 7.314- 7.960 mg/g, respectively. CONCLUSIONS The established method has high sensitivity and good reproducibility, and can provide reference for the quality control of the preparation.

15.
China Pharmacy ; (12): 1199-1203, 2023.
Article in Chinese | WPRIM | ID: wpr-973619

ABSTRACT

OBJECTIVE To establish the method for content determination of related substances in Oxcarbazepine tablets. METHODS Ultra-high performance liquid chromatography (UPLC) method was adopted and the separation was performed on ZORBAX Eclipse Plus C18 column with mobile phase consisted of acetonitrile-0.01 mol/L ammonium acetate solution (pH6.0) (gradient elution) at the flow rate of 0.5 mL/min. The detection wavelength was 230 nm and column temperature was set at 35 ℃. The sample size was 10 μL. RESULTS The linear ranges of oxcarbazepine and impurity A, B, C, D, E, I, K, L and N were 0.192-1.440, 1.019-7.639, 0.208-1.559, 0.230-1.727, 0.389-2.915, 0.182-1.364, 0.393-2.945, 0.199-1.493, 0.199-1.490 and 0.200- 1.503 μg/mL, respectively (all r>0.999). The detection limits were 0.046, 0.037, 0.049, 0.027, 0.077, 0.040, 0.114, 0.054, 0.055 and 0.039 μg/mL. The quantitation limits were 0.152, 0.122, 0.162, 0.090, 0.258, 0.132, 0.380, 0.181, 0.185 and 0.130 μg/mL. RSDs of precision, repeatability, stability (24 h) and durability tests were all lower than 5.0%. The average recoveries were 92.8%-105.6% (RSD≤3.0%, n=9). Only impurity K and unknown impurity were detected in the original preparation sample, with a total content of 0.078% to 0.083%; impurities A, B, D, I and unknown impurity were detected in the generic preparations produced by domestic enterprise Ⅰ, with a total content of 0.147% to 0.163%; impurities A, B, I and unknown impurity were detected in the generic preparations produced by domestic enterprise Ⅱ, with a total content of 0.085% to 0.161%. CONCLUSIONS The established method is rapid, sensitive, accurate, stable and durable. It can be used for the content determination of 9 known impurities in Oxcarbazepine tablets.

16.
China Pharmacy ; (12): 802-806, 2023.
Article in Chinese | WPRIM | ID: wpr-969575

ABSTRACT

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.

17.
China Pharmacy ; (12): 2328-2332, 2023.
Article in Chinese | WPRIM | ID: wpr-996387

ABSTRACT

OBJECTIVE To provide a reference for comprehensive quality evaluation and control of the effective parts of Dracocephalum moldavica (EPDM). METHODS A total of 10 batches of EPDM were prepared, and chemical information of EPDM was collected by HPLC-Q-Exactive-MS. EPDM components were identified by literature search, database comparison and manual analysis. HPLC fingerprints of 10 batches of EPDM were established by using the Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprint (2004 A edition); the similarity evaluation and common peak identification were carried out, and the contents of 5 index components were determined by HPLC. RESULTS A total of 11 compounds in EPDM were identified. The fingerprint similarities of EPDM samples from 10 batches were all above 0.96. Among 11 chromatographic peaks, 5 peaks were identified, such as luteolin-7-O-β-D-glucuronide(LG), apigenin-7-O-glucuronide(APG), rosmarinic acid(RA), diosmetin-7-O-β-D-glucuronide(DG), tilianin(TL) . The results of the quantitative analysis showed that all above 5 components had good linearity (R2≥0.999), and the average recoveries were in the range of 95.12%-98.37%. The contents of LG, APG, RA, DG, TL were 21.268 3-29.243 9, 6.365 4-7.771 7, 37.327 4-45.671 2, 17.169 9-21.985 9, 66.940 4-91.206 3 mg/g, respectively. CONCLUSIONS The established method of component identification, fingerprint and content determination is stable, feasible and reliable, which is suitable for the comprehensive quality evaluation and control of EPDM.

18.
China Pharmacy ; (12): 2198-2203, 2023.
Article in Chinese | WPRIM | ID: wpr-988777

ABSTRACT

OBJECTIVE To establish methods to identify the chemical components of Gantaishu capsule, and determine the contents of 6 index components including glycyrrhizic acid. METHODS The chemical components of Gantaishu capsule were determined by HPLC-TOF/MS; the contents of 6 index components including glycyrrhizic acid were determined by UPLC-MS/MS. RESULTS A total of 41 chemical components were identified in Gantaishu capsules. The linear ranges of glycyrrhizic acid, mangiferin, luteolin, costunolide, oleanolic acid and berberine were 200-10 000 ng/mL(r were all greater than 0.999). The limits of quantification were 200, 20, 10, 1, 10, 0.5 ng/mL, and the limits of detection were 100, 10, 5, 0.5, 5, 0.25 ng/mL, respectively; RSDs of precision, stability (24 h) and reproducibility tests were all less than 5.0% (n=6 or n=3); the recoveries were 99.05%-101.08% (RSD were all less than 2.0%, n=6). The contents of them were 2.42-2.66, 0.85-1.16, 0.35-0.46, 6.18- 6.46, 0.99-1.29, 5.22-5.56 mg/g. CONCLUSIONS The established methods for identification and content determination are rapid and simple, and can be used for the identification of chemical components and the content determination of index components in Gantaishu capsule.

19.
Journal of Pharmaceutical Practice ; (6): 552-556, 2023.
Article in Chinese | WPRIM | ID: wpr-988639

ABSTRACT

Objective To establish a gas chromatography for simultaneous determination of camphor residue and borneolum content in Qingchang Suppository. Methods Gas chromatograph method was used. The chromatographic column was Agilent capillary column(30 m×0.25 mm×0.25 µm). The column temperature was 140 ℃. The sample injection temperature was 250 ℃. The FID detector temperature was 250 ℃. Results Camphor,borneol and isoborneol content showed good linear in the extent of 0.0299~1.497(r=1.000), 0.0205~1.025(r=1.000), 0.0097~0.4830 µg (r=1.000). RSDs of precision,stability and repeatability test results were less than 2%. The recovery was 99.7%, 101.0%, 102.5%. Conclusion This method is simple and quick with accurate result, which could be used for the content determination of Borneol in Qingchang Suppository.

20.
Chinese Journal of Experimental Traditional Medical Formulae ; (24): 134-140, 2023.
Article in Chinese | WPRIM | ID: wpr-988189

ABSTRACT

ObjectiveTo investigate the effect of microemulsion on the distribution of index components in different phases of Zexietang extract based on high performance liquid chromatography(HPLC) and phase separation process. MethodParticle size meter and transmission electron microscope were used to characterize the colloidal particles in blank microemulsion, aqueous extract of Zexietang and microemulsion extract of Zexietang. The phase separation process was established by high-speed centrifugation and dialysis, and based on this process, the aqueous extract and microemulsion extract of Zexietang were separated into the true solution phase, the colloidal phase and the precipitation phase, respectively. The contents of six components, including atractylenolide Ⅲ, atractylenolide Ⅱ, 23-acetyl alisol C, alisol A, alisol B and alisol B 23-acetate, were determined by HPLC with the mobile phase of water(A)-acetonitrile(B) for gradient elution(0-5 min, 40%-43%B; 5-20 min, 43%-45%B; 20-45 min. 45%-60%B; 45-75 min, 60%-80%B). The solubility of the index components in water and microemulsion was determined by saturation solubility method. ResultThe colloidal particles in the aqueous extract, microemulsion extract and blank microemulsion were all spherical, and the particle size, polydispersity index(PDI) and Zeta potential of the colloidal particles were in the order of aqueous extract >microemulsion extract >blank microemulsion. The results of phase separation showed that the colloidal phase and the true solution phase could be completely separated by dialysis for 2.5 h, and the phase separation process was tested to be stable and feasible. Compared with the aqueous extract of Zexietang, the use of microemulsion as an extraction solvent could increase the contents of atractylenolide Ⅲ, 23-acetyl alisol C, atractylenolide Ⅱ , alisol A, alisol B and alisol B 23-acetate by 3.75, 6.82, 35.47, 10.66, 35.41, 27.75-fold, and could increase the extraction efficiencies of the latter five constituents by 2.03, 1.15, 1.70, 6.43, 5.53 times. The solubility test showed that the microemulsion could significantly improve the solubility of atractylenolide Ⅱ, alisol A, alisol B and alisol B 23-acetate, but it had less effect on the solubility of atractylenolide Ⅲ and 23-acetyl alisol C. ConclusionMicroemulsion can improve the extraction efficiency and increase the distribution of the index components in the colloidal phase state of Zexietang to different degrees, providing a reference for the feasibility of microemulsion as an extraction solvent for traditional Chinese medicine.

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