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1.
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.

2.
Article in Chinese | WPRIM | ID: wpr-846650

ABSTRACT

Objective: To isolate and identify the terpenoids from the aerial parts of Gendarussa vulgaris. Methods: The 95% EtOH extract of the aerial parts of G. vulgaris were isolated and purified by silica gel, Sephadex LH-20, reversed-phase ODS, macroporous adsorption resin AB-8 and semi-preparative high performance liquid chromatography. The compound structures were identified by physicochemical properties and spectroscopic data. Results: Ten terpenoids were identified as gvterpennoid A (1), 4,4,14α- trimethylpregn-8-en-3β,20α-diol (2), betulone (3), ergosterol endoperoxide (4), ursolic acid (5), oleanolic acid (6), 3β-hydroxyl- 11α,12α-epoxy olean-28,13β-lactone (7), sweroside (8), loganin (9), and dehydromorroniaglycone (10). Conclusion: Compound 1 is a new triterpene, named gvterpennoid A. Compound 2 is a new natural product, and its 13C- and 1H-NMR chemical shifts were first completely assigned on the basis of 1D and 2D NMR spectroscopic evidence. Compounds 3-5, 7-10 are isolated from Gendarussa genus for the first time.

3.
Article in Chinese | WPRIM | ID: wpr-846568

ABSTRACT

Objective: To screen the differential ingredients between crude and wine-processed Corni Fructus and determin their content. Methods: An integrated strategy using ultra performance liquid chromatography coupled with tandem quadrupole time-of- flight mass spectrometry (UPLC-Q-TOF/MS) and the chemometric approach was applied to compare the global chemical profile of crude and wine-processed Corni Fructus. Then, the main differential ingredients were quantified by UPLC-PDA. Results: The chemical profiling of wine-processed Corni Fructus was significantly different. Ten compounds could be considered as characteristic chemical markers for distinguishing crude and wine-processed Corni Fructus, including 5-hydroxymethyl furfuraldehyde (5-HMF), gallic acid, protocatechuic acid, morroniside, loganic acid, sweroside, cornin, dihydroquercetin, loganin and cornoside. A new UPLC-PDA quantitative method for analyzing simultaneously the above ten compounds in wine-processed Corni Fructus was established. The results of methodology investigation showed that the ten components were well linear within the investigation range (r ≥ 0.999 7). Compared with the crude Corni Fructus, the content of seven components were increased, including gallic acid, 5-HMF, loganin, morroniside, cornin, sweroside and dihydroquercetin, and the other three components in wine-processed Corni Fructus were decreased. Conclusion: The differential ingredients obtained by chemometric-based approach can be used to distinguish crude and wine-processed Corni Fructus. The determination method of wine-processed Corni Fructus established is accurate and reliable, which can be used for the quality control of Corni Fructus.

4.
Article in Chinese | WPRIM | ID: wpr-846560

ABSTRACT

Objective: To establish a quick method of ultra-performance liquid chromatography-quadrupole time-of-fight mass spectrometry (UPLC-Triple-TOF/MS) for the analysis of components of crude and sweated Dipsaci Radix. Methods: The separation was performed on the chromatographic column of Agilent Eclipse XDB-C18 (250 mm × 4.6 mm, 5.0 μm), and the mobile phase was 0.1% formic acid solution-methanol, with a gradient elution at a flow rate of 0.8 mL/min, the detection wavelength was 215 nm, the column temperature was 25 ℃. UPLC-Triple-TOF 5600+ time of flight liquid and mass spectrometer was used for mass spectrometry. Electrospray ion source negative ion mode was adopted, and the scanning range was m/z 100-1 500. The components of crude and sweated Dipsaci Radix were quickly identified according to the information obtained by high-resolution mass spectrometry combined with secondary mass spectrometry. Results: Fifty-two common components were identified or tentatively characterized based on the retention time and MS spectra. They were triterpenoid saponins, iridoids, phenolic acids etc. The crack rules of primary components were also analyzed. And comparing the components of crude and sweated Dipsaci Radix, it showed that the content of 20 components such as loganin acid, chlorogenic acid, loganin, isochlorogenic acid A, and asperosaponin VI was decreased after sweating, and caffeic acid, isochlorogenic acid, isochlorogenic acid C, and triplostoside A was increased. Conclusion: The types of components of crude and sweated Dipsaci Radix are identical, but there are differences in the content of the components. The content of the components of crude are higher than the sweated Dipsaci Radix. UPLC-Triple-TOF-MS technology was used to analyze the influence of “sweating” on the chemical composition of the Dipsaci Radix, so as to provide a theoretical basis for the study of the chemical constituents of sweated Dipsaci Radix and further research on the origin processing of Dipsaci Radix.

5.
Article in Chinese | WPRIM | ID: wpr-846425

ABSTRACT

Objective: Taking Qiju Dihuang Pills (QDP) as the research object, time domain reflection method was used for real-time determination of moisture content in concentrated pills during drying process and optimization of the drying process parameters. Methods: The moisture model of the drying process of QDP was established by the relationship between the water, temperature, and the reflective signal value of time domain reflector. The effect of the drying process on the different thickness (8, 16, and 24 mm), different drying temperatures (30, 40, 50, 60, 70, 80, and 90℃) was investigated. Results: The moisture model of the drying process of QDP was measured by time domain reflection method as Y = 0.305 X-34.772 (r2 = 0.999); X = X(T)-(0.768 9 T-24.824 7) (T ≥ 30℃). The optimized process was as following: the process was dried at 60℃ to 13.8% moisture and then rising to 80℃, after being dried to 7.80%, cooled to 60℃ and dried to 5.0% target moisture. Conclusion: It is feasible to test the moisture content in the drying process of QDP by time domain reflection method. This method can be used to monitor and popularize the moisture content in the drying process of traditional Chinese medicine concentrated pills.

6.
Article in Chinese | WPRIM | ID: wpr-846388

ABSTRACT

Objective: To establish an HPLC fingerprint of Qingxin Zishen Prescription Decoction (QZPD) and determine the contents of its multiple components, so as to provide a scientific basis for quality control. Methods: HPLC analysis was performed on a Phenomenex Kinetex C18 column (100 mm × 4.60 mm, 2.6 μm) for gradient elution with the mobile phase consisting of methanol, acetonitrile and 0.2% formic acid aqueous. The detection wavelength was set at 245 nm and 280 nm, and the column temperature was 40 ℃. Fingerprints of ten batches of QZPD were determined, and the similarities among fingerprints were evaluated. Attributive analysis and identification of common peaks were performed and the contents of 15 components were determined. Results: The fingerprint similarities of 10 batches of QZPD were ranged from 0.923 to 0.998 compared with the reference fingerprint, and 33 common peaks were identified in the fingerprint. Among them, seven peaks (P11, P14-P16, P24, P29, P30) were identified from Coptidis Rhizoma, two peaks (P7, P19) were identified from Nelumbinis Plumula, two peaks (P14, P21) were identified from Ziziphi Spinosae Semen, nine peaks (P4, P5, P10, P17, P18, P28, P31-P33) were identified from Salvia miltiorrhiza, nine peaks (P1-P3, P6, P8, P9, P12, P13, P20) were identified from Corni Fructus, while five peaks (P22, P23, P25-P27) cannot be originated and none of the common peaks was identified from Rehmanniae Radix, Uncariae Ramulus Cum Uncis and Triticum aestivum. By comparing with the chemical reference, fifteen components, including gallic acid (P2), 5-hydroxymethylfurfural (P3), danshensu (P4), protocatechuic aldehyde (P5), morroniside (P9), caffeic acid (P10), cornin (P12), loganin (P13), magnoflorine (P14), coptisine (P24), lithospermic acid (P28), berberine (P29), palmatine (P30), salvianolic acid B (P31) and salvianolic acid E (P33), were identified and quantified. The contents of the fifteen components were 158.3-248.2, 233.6-321.3, 45.9-166.0, 24.3-38.6, 800.7-1 263.6, 26.6-54.9, 44.5-108.2, 470.4-757.3, 85.6-178.6, 11.1-34.2, 56.2-106.4, 25.9-138.9, 21.0-59.2, 951.6-2 244.7 and 38.6-92.8 μg/g, respectively. Conclusion: The method established in this study is stable and highly reproducible, and can provide basis for quality control of QZPD.

7.
Article in Chinese | WPRIM | ID: wpr-846233

ABSTRACT

Objective: To establish a scientific and reasonable quality control method of Bufei Granules through the qualitative and quantitative research of thin layer identification and content determination of Bufei Granules. Methods: Based on the main chemical constituents of each drug in Bufei Granules, TLC method was used to analyze Corni Fructus, Ephedrae Herba, Paeoniae Radix Rubra, Scutellariae Radix, Citri Reticulatae Pericarpium, and Glycyrrhizae Radix et Rhizoma; HPLC was used to determine the content of loganin and baicalin. The content of loganin was analyzed by Agilent Eclipse XDB-C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of acetonitrile-methanol-water-formic acid (10:1:89:0.1). The detection wavelength was set at 236 nm; The content of baicalin was analyzed by Dikma Diamonsil C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of methanol-water-formic acid (49:51:0.1). The detection wavelength was set at 280 nm. Results: The TLC identification method can distinguish Ephedrae Herba, Paeoniae Radix Rubra, Scutellariae Radix, Citri Reticulatae Pericarpium, and Glycyrrhizae Radix et Rhizoma with clear spots, no negative interference, good separation and strong specificity. Loganin and baicalin were used as index components in methodological study. The average recovery of loganin was 98.49% and the RSD was 0.80%; The repeatability test RSD was 0.83% which met the requirement. The linear range was from 4.76 μg/mL to 50.70 μg/mL and the linear relationship was good (r = 0.999 9). The average recovery of baicalinrate was 101.20% and the RSD was 0.77%. The repeatability test RSD was 0.90%, which met the requirements. The linear range was from 6.00 μg/mL to 96.00 μg/mL and the linear relationship was good (r = 0.999 9). The loganin content of three bantches of samples was 12.04, 9.78 and 11.81 mg/bag; And the content determination result of baicalin was 121.13, 101.31 and 103.14 mg/bag. Conclusion: The method is easy to operate, strong in specificity, accurate and sensitive, with good repeatability. It can be applied for the quality control of Bufei Granules.

8.
China Pharmacy ; (12): 2508-2511, 2020.
Article in Chinese | WPRIM | ID: wpr-829359

ABSTRACT

OBJECTIVE:To estab lish a me thod for simultaneous determination of morroniside ,loganin,echinacoside and acteoside in Huanshao capsules. METHODS :HPLC method was adopted. The determination was performed on Zhongpuhong RD-C18 column with mobile phase consisted of acetonitrile- 0.1% formic acid solution (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelength was set at 240 nm (morroniside,loganin) and 330 nm (echinacoside,acteoside). The column temperature was set at 35 ℃,and sample size was 10 μL. RESULTS:The linear range were 5.29-105.80 μg/mL for morroniside, 4.49-89.88 mg/L for loganin ,16.26-325.25 mg/L for echinacoside and 16.31-326.25 mg/L for acteoside ,r values were 0.999 9. RSDs of precision ,stability (24 h),reproducibility and durability tests were all lower than 2.0% . The recoveries were 94.34% -96.23%(RSD=0.81% ,n=6),97.04% -98.89%(RSD=0.73% ,n=6),96.23% -98.08%(RSD=0.82% ,n=6), 95.40%-98.47%(RSD=1.23%,n=6),respectively. The contents of above 4 components in 11 batches of Huanshao Capsules were 0.190-0.704,0.439-0.857,2.723-4.475 and 0.589-1.035 mg/g,respectively. CONCLUSIONS :Established method is specific , precise and can be used for content determination of 4 components in Huanshao capsules.

9.
China Pharmacy ; (12): 782-788, 2020.
Article in Chinese | WPRIM | ID: wpr-819087

ABSTRACT

OBJECTIVE:To study the effects of loganin on the prolife ration and apoptosis of liver cancer HepG 2 cells,and to explore its mechanism. METHODS :CCK-8 assay was used to detect the effects of different concentrations (10,25,50,100, 150,200,300,400 µg/mL)of loganin on the proliferation activity of HepG 2 cells for 24 and 48 h. HepG 2 cells were divided into control group ,loganin low-concentration ,medium-concentration and high-concentration groups (50,100,150 μ g/mL). After treated for 24 h,morphological changes of apoptosis of cells were detected by Hoechst 33342 fluorescence staining. The apoptosis and cycle distribution of cells were detected by flow cytometry. Western blotting was used to detect protein expression of Cyclin D1, PCNA, Bcl-2, Caspase-3, Cleaved-Caspase-3, Caspase-9 and Cleaved-Caspase- 9. RESULTS : Loganin inhibited the proliferation of HepG 2 cells,in concentration-dependent trend. Compared with control group ,apoptosis as pyknosis and fragmentation occurred ,and the apoptosis rate increased significantly in loganin low-concentration ,medium-concentration and high-concentration groups (P<0.01);the cell were mainly blocked in S phase ;relative protein expression of Cyclin D 1,PCNA and Caspase- 3 were significantly decreased ,while that of Cleaved-Caspase- 3 were significantly increased in loganin low- concentration, medium-concentration and high-concentration groups (P<0.05 or P<0.01); relative protein expression of Cleaved-Caspase-9 were increased significantly ,while that of Bcl- 2 and Caspase- 9 were decreased significantly in loganin medium-concentration and high-concentration groups (P<0.05 or P<0.01). CONCLUSIONS :Loganin can significantly inhibit the proliferation and induce apoptosis of HepG 2 cells,the mechanism of which may be associated with inhibiting Bcl- 2 protein expression and promoting Caspase- 3,Caspase-9 activation.

10.
Article in Chinese | WPRIM | ID: wpr-851334

ABSTRACT

Objective: To establish a rapid, accurate, and practical HPLC method for simultaneous determination the content in Qiju Dihuang Oral Liquid (QDOL) of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol. Methods: YMC ODS column (250 mm × 4.6 mm, 5 μm) was used, column temperature was set at 35 ℃, gradient elution with 0.1% formic acid aqueous solution- acetonitrile was used as mobile phase, flow rate was 1.0 mL/min, detection wavelength was 254 and 325 nm. The injection volume was 10 μL. Results: The injection amount of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, paeonol injection quality at 0.08—1.60, 0.12—2.40, 0.09—1.80, 0.06—1.20, 0.10—2.00, 0.30—6.00, 0.01—0.20, 0.01—0.20, 0.01—0.20, 0.005—0.10, 0.005—0.10, and 0.01—0.20 μg showed a good linear relationship with peak area, with good precision, repeatability and stability. The recovery rates of the samples were between 96% and 103%, the RSD was 2.13%, 3.45%, 2.86%, 2.59%, 3.15%, 3.49%, 2.19%, 3.25%, 2.37%, 2.53%, 2.91%, and 3.35%, respectively. The content of each component of the five batches of samples was stable, and the mass concentrations range of the 12 components tested were 98.56—102.56, 204.28—212.10, 18.53—18.89, 1.95—2.05, 12.31—12.54, 87.01—87.12, 5.35—5.43, 16.08—16.15, 8.69—8.72, 8.89—8.95, 5.12—5.19, and 1.87—1.94 μg/mL. Conclusion: The method simltaneosly determines the content of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol in QDOL, which is suitable for the quality control of QDOL.

11.
Article in Chinese | WPRIM | ID: wpr-851059

ABSTRACT

Objective: To compare the differences in pharmacokinetic behavior of six ingredients in Qikui Sustained-release Tablets in rabbit plasma. Qikui Granules was taken as reference. Methods: Diazepam was used as internal standard. LC-MS/MS detection methods of astragaloside, hyperin, isoquercitrin, rutin, morroniside, and loganin in rabbit plasma were established, and pharmacokinetic parameters of six components were calculated. Results: Six active ingredients’ equation of linear regressions were: astragaloside Y = 1.0 × 10-4 X - 0.009 9 (r = 0.999 7), morroniside Y = 1.0 × 10-4 X + 0.038 7 (r = 0.999 4), loganin Y = 3.0 × 10-5 X + 0.008 7 (r = 0.999 3), hyperin Y = 1.0 × 10-3 X - 0.016 1 (r = 0.999 0), rutin Y = 5.0 × 10-4 X - 0.011 5 (r = 0.999 4), isoquercitrin Y = 1.7 × 10-3X - 0.307 5(r = 0.999 2). Intra-day and inter-day precision and accuracy and recovery rate were up to the mustard. After Qikui Sustained-release Tablets and Qikui Granules being given by gavege, the maximal concentration (Cmax) of morroniside, loganin, astragaloside, rutin, hyperin, and isoquerctirin in Qikui Granules were (1.333 ± 0.051), (1.238 ± 0.164), (0.83 ± 0.079), (0.127 ± 0.017),(0.444 ± 0.048), and (0.223 ± 0.048) mg/L, t1/2 were (3.848 ± 0.311), (3.822 ± 0.757), (4.982 ± 1.14), (3.73 ± 0.298), (4.732 ± 0.642), and (5.132 ± 0.901) h, respectively, AUC(0-t) were (3.069 ± 0.307), (2.891 ± 0.943), (2.079 ± 0.306), (0.313 ± 0.068), (1.087 ± 0.177), (0.496 ± 0.129) mg∙h/L, respectively, Cmax of morroniside, loganin, astragaloside, rutin, hyperin, and isoquerctirin in Qikui Sustained-release Tablets were (0.985 ± 0.13), (0.961 ± 0.175), (0.693 ± 0.101), (0.094 ± 0.012), (0.354 ± 0.045), (0.201 ± 0.037) mg/L, t1/2 were (4.691 ± 0.337), (5.62 ± 1.64), (6.408 ± 0.707), (4.103 ± 0.341), (6.048 ± 0.882), (5.803 ± 0.59) h, AUC(0-t) were (5.191 ± 1.046), (6.168 ± 1.25), (4.293 ± 0.823), (0.485 ± 0.103), (1.84 ± 0.432), (0.924 ± 0.19) mg∙h/L. Contrast with Qikui Granules, relative bioavailability of morroniside, loganin, astragaloside, rutin, hyperin, and isoquerctirin in Qikui Sustained-release Tablets were 169.1%, 213.3%, 206.5%, 156.0%, 169.3%, and 186.3%, respectively. Conclusion: Qikui Sustained-release Tablets can significantly improve the bioavailability of each active ingredient in rabbit.

12.
Article in Chinese | WPRIM | ID: wpr-850926

ABSTRACT

Objective: To study the spectrum-effect relationships of fingerprints of sweated and crude Dipsaci Radix on cell proliferation and differentiation, and find out the material basis of efficacy before and after sweating in order to provide the basis for the impact of the efficacy. Methods: The DAD detector was used to establish HPLC fingerprints of sweated and crude Dipsaci Radix, and the relationship between the spectrum and efficiency was established by gray relational analysis. Results: The chemical composition of peaks 14 and 4 were highly correlated with the proliferation and differentiation of osteoblasts and the proliferation of MG-63 cells. The correlations were all above 0.7. The three pharmacophore indicators associated much with the characteristic peaks 14, 4, 6, 16, 13, 11, and 5. Combined with the previous analysis, these peaks represented respectively asperosaponin VI, chlorogenic acid, loganin, asperosaponin IV isomers, dipsacoside X, chlorogenic acid C, and caffeic acid. Conclusion: Asperosaponin VI, chlorogenic acid, loganin, asperosaponin IV isomers, dipsacoside X, chlorogenic acid C, and caffeic acid may be the main material basis for the effect of cell proliferation and differentiation, thus affecting its efficacy.

13.
Article in Chinese | WPRIM | ID: wpr-850857

ABSTRACT

Objective: To study Lonicerae Japonicae Flos, Lonicerae Japonicae Caulis, and Lonicerae Japonicae Leaves by UPLC method, and study the different parts of Lonicera japonica by the fingerprint similarity evaluation, cluster analysis, principal component analysis, and other chemical pattern recognition technologies, in order to provide scientific basis for the comprehensive utilization of L. japonica. Methods: The method was carried out on an ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) by a gradient elution using acetonitrile and 0.1% phosphoric acid. The flow rate was 0.3 mL/min, The column temperature was 30 ℃. The sample room temperature was 8 ℃. The detection wavelengths were 326, 238, and 250 nm, and the injection volume was 1 μL. Results: The UPLC fingerprint of 28 batches of samples from different parts of Lonicerae Japonicae were set up and 14 common peaks were obtained. They were new chlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, loganin, rutinum, luteoloside, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C. There were some differences in chemical composition and quantity of Lonicerae Japonicae Flos, Lonicerae Japonicae leaves, and Lonicerae Japonicae Caulis. PCA and cluster analysis revealed the similarity and difference of 28 batches of samples from different parts of L. japonica. Conclusion: The combination of clustering analysis and principle component analysis could be used to confirm that the chemical constituents of Lonicerae Japonicae Flos and Lonicerae Japonicae leaves were similar, but there was a difference between Lonicerae Japonicae Flos and Lonicerae Japonicae Caulis. The established fingerprint method can provide a reference for the quality control of Lonicerae Japonicae Flos, Lonicerae Japonicae leaves, and Lonicerae Japonicae Caulis.

14.
China Pharmacy ; (12): 1203-1209, 2019.
Article in Chinese | WPRIM | ID: wpr-816964

ABSTRACT

OBJECTIVE: To establish the method for the rapidly non-destructive quality control of Liuwei dihuang capsule. METHODS: AOTF-NIR spectrometry was adopted. Taking 80 batches of Liuwei dihuang capsule produced by a manufacturer in recent three years as samples, HPLC chromatogram was adopted to determine the contents of loganin, morroniside, paeonol, paeoniflorin and ursolic acid; the content of water was determined according to general principles stated in 2015 edition of Chinese Pharmacopeia (part Ⅰ). Taking 70 batches of samples as correction set, the partial least square method and the cross-validation algorithm were used to establish the NIR quantitative model of 6 indexes in Liuwei dihuang capsules with the Unscrambler quantitative analysis software. Taking residual 10 batches of samples as validation set, external validation was conducted for the model. RESULTS: The correlation coefficients (R2) of internal and external validation of loganin, morroniside, paeonol, paeoniflorin, the content of water quantitative model were all greater than 0.9; the correction of standand deviation (RMSEC) were 0.372 8, 0.025 4, 0.263 3, 0.288 5, 0.186 7 and 0.037 7; the prediction of standard deviation (RMSEP) were 0.462 2, 0.077 5, 0.472 1, 0.634 9, 0.293 4 and 0.206 9; the external verification showed that mean deviations of preclicted value to actual value were 6.04%, 6.05%, 5.87%, 6.97%, 5.62% and 4.83%, with the mean deviation less than 10%.CONCLUSIONS:The established method can achieve rapidly non-destructive analysis Liuwei dihuang capsule.

15.
Chinese Traditional Patent Medicine ; (12): 1093-1096, 2018.
Article in Chinese | WPRIM | ID: wpr-710275

ABSTRACT

AIM To establish an HPLC method for the simultaneous content determination of chlorogenic acid,loganin,paeoniflorin,baicalin,salvianolic acid B and paeonol in Tuiyin Mixture (Moutan Cortex,Paeoniae Radix Rubra,Lonicerae japonicae Caulis,etc.).METHODS The analysis of methanol extract of this drug was performed on a 30 ℃ thermostatic ZORBAX SB-Aq column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1% phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 235 nm.RESULTS Six constituents showed good linear relationships within their own ranges (r≥0.999 7),whose average recoveries were 97.1%-100.6% with the RSDs of 1.35%-2.28%.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of Tuiyin Mixture.

16.
Article in Chinese | WPRIM | ID: wpr-710250

ABSTRACT

AIM To establish an HPLC-DAD method for the simultaneous content determination of six constituents in Maiwei Dihuang Pills (Ophiopogonis Radix,Schisandrae chinensis Fructus,Rehmanniae Radix Praeparata,etc.).METHODS The analysis of 50% methanol extract of this drug was performed on a 35 ℃ thermostatic Agilent ZORBAX SB-C18column (4.6 mm × 150 mm,5 μm),with the mobile phase comprising of acetonitrile-water (containing 0.2% phosphate acid) flowing at 0.8 mL/min in a gradient elution manner,and the detection wavelengths were set at 220,230,236 and 274 nm.RESULTS Deoxyschizandrin,schizandrin B,schisandrin,paeoniflorin,paeonol and loganin showed good linear relationships within the ranges of 10-70,6.5-45.5,33.5-234.5,17-119,31-217 and 34-238 μg/mL (r >0.990 0),whose average recoveries (RSDs) were 99.6% (1.7%),100.4% (1.8%),100.7% (1.8%),102.9% (1.7%),102.2% (1.5%) and 99.7% (1.2%),respectively.CONCLUSION This simple and reproducible method can be used for the rapid quality control of Maiwei Dihuang Pills.

17.
Article in Chinese | WPRIM | ID: wpr-707160

ABSTRACT

Objective To establish an HPLC method for the content determination of morroniside, sweroside, paeoniflorin and loganin of Liuwei Dihuang Decoction and its Cornus Officinalis-Cortex Moutan couple; To discuss the relationship between the whole prescription and the couple of main pharmacodynamic components. Methods The HPLC method was used at Hypersile C18 column (4.6 mm × 250 mm, 5 μm); the mobile phase consisted of methanol-water (24:76); the detective wavelength was 236 nm; the flow rate was 1.0 mL/min; the column temperature was 30 ℃. Results The linear ranges of morroniside, sweroside, paeoniflorin and loganin were among 0.480–7.680 μg (r=0.999 3), 0.103–1.650 μg (r=0.999 5), 0.120–1.920 μg (r=0.999 1) and 0.227–3.630 μg (r=0.999 7), respectively. The average recovery rates and RSD were 102.79%, 102.29%, 100.99%, 102.48%, and 1.73%, 1.48%, 1.32%, 0.75%, respectively. The contents of morroniside, sweroside and paeoniflorin in Liuwei Dihuang Decoction were slightly higher than that in Cornus Officinalis - Cortex Moutan couple, and the contents of loganin were almost the same. Conclusion The method is simple, stable, accurate and reproducible. It can be used for content determinate of glycosides in Liuwei Dihuang Decoction and Cornus Officinalis-Cortex Moutan couple. Cornus Officinalis-Cortex Moutan couple has the glycosides with tonifying kidney effect of Liuwei Dihuang Decoction.

18.
Article in Chinese | WPRIM | ID: wpr-687371

ABSTRACT

To establish the HPLC fingerprint and determine five index components (loganic acid, chlorogenic acid, loganin, sweroside and asperosaponin Ⅵ) of Zishen Yutai pills by high performance liquid chromatography, and provide a scientific basis for its quality control. The fingerprint chromatogram was analysed by the chromatographic fingerprint similarity evaluation system for tradition Chinese medicine (2012), fifteen common peaks were obtained at the wavelength of 254 nm. Different batches of Zishen Yutai pills showed a similarity of above 0.90 in HPLC fingerprint profiles. For the quantitive analysis method, The separation of five components showed good regression (>0.999 2) with linear ranges, and the mean recoveries were in the range of 97.62%-101.9%, with the RSD (=9) less than 3%. The established fingerprint and quantitative analysis methods are highly specific, simple and accurate, which can reflect the quality of Zishen Yutai pills more comprehensively, and can be used for its quality control.

19.
Article in Chinese | WPRIM | ID: wpr-851752

ABSTRACT

Objective To study the chemical constituents from the leaf of Syringa oblata. Methods The compounds was isolated by silica gel column chromatography and HPLC, and their structure were identified by spectral data analysis. Results A total of 35 compounds were isolated and identified as oleanolic acid (1), ursolic acid (2), betulinic acid (3), 1,3-benzodioxole-5-propanol (4), p-hydroxyl benzene propyl alcohol (5), p-hydroxyl benzene ethel alcohol (6), syringopicrogenin D (7), syringopicrogenin E (8), syringopicrogenin F (9), syringopicrogenin A (10), syringopicrogenin C (11), 3,4-dihydroxyl benzene ethel alcohol (12), syringobittergenin B (13), syringo-picrogenin B (14), grasshopper ketone (15), (7R,8S)-4,9,9’-trihydroxyl-3,3’-dimethoxyl-7,8- dihydrobenzofuran-1’-propylneolignan (16), lariciresinol (17), syringin (18), 3(Z)-enol glucoside (19), quercetin-3-O-β-D- glucopyranoside (20), (8E)-ligstroside (21), epipinoresinol-4-O-β-D-glucopyranoside (22), (8E)-ligstroside B (23), (8E)-ligstroside A (24), salidroside (25), 7-dehydrologanin (26), fliederoside B (27), syringopicroside B (28), oleoside dimethyl ester (29), lilacoside (30), syrigopicroside (31), oleuropein (32), (+)-lariciresinol-4-O-β-D-glucopyranoside (33), verbascoside (34), and (+)- epipinoresinol-4’-O-β-D-glucopyranoside (35). Conclusion Compounds 4, 5, 14-16, 19, 23, 24, 26, and 27 are isolated from S. oblata for the first time.

20.
Article in Chinese | WPRIM | ID: wpr-851479

ABSTRACT

Objective To establish HPLC fingerprint strategy to simultaneously determine nine components in Liver-protection Agent, including loganin, paeonflorin, scutellarin, baicalin, baicalein, deoxyschizandrin, schisandrin, schizandrin C, and ursolic acid, and provide a scientific basis for the quality control of Liver-protection Agent and related medicinal preparations. Methods The analytical analysis was performed on an Agilent 1260-HPLC system equipped with a VWD detector and SB-C18 reversed phase column (Zorbax 150 mm × 4.6 mm, 5 μm). The analytes were eluted using a gradient mixture of two solvent: solvent A was distilled deionized water containing 0.1% ortho-phosphoric acid and solvent B was 100% acetonitrile. The mobile phase flow rate was 1.0 mL/min. The separation temperature was 30 ℃. The detection wavelengths were 236, 280, and 210 nm. The injection volume was 5 μL. Common patterns of HPLC fingerprints for 10 batches of Liver-protection Agent medicinal preparations were established, and chemometric analysis method was employed to analyze the hidden information. At the same time, methodological study was conducted for determinations of multiple components including loganin, paeonflorin, scutellarin, baicalin, baicalein, deoxyschizandrin, schisandrin, schizandrin C, and ursolic acid. Results The HPLC fingerprint strategy of Liver-protection Agent medicinal preparation had been set up, and 37 common peaks had been identified with the similarity of more than 0.9. Moreover, the samples were roughly divided into four categories by the methods of the systematic cluster analysis and principle component analysis. After validating the multiple component quantitative analysis condition through methodology, the average recovery rate was between 95.13% and 104.8%.The average mass concentration of loganin, paeonflorin, scutellarin, baicalin, baicalein, deoxyschizandrin, schisandrin, schizandrin C, and ursolic acid in ten batches of Liver-protection Agent was 216.3-223.0, 126.1-137.1, 144.7-149.0,1 623.1-1 992.7, 481.9-520.0, 14.9-18.7, 33.8-37.0, 2.9-3.7, and 39.7-43.6 mg/L, respectively. Conclusion The combination methods of HPLC fingerprint and simultaneous determinations of multiple components are rapid, simple, and reproducible, which can be adopted as one of the quality control methods for Liver-protection Agent and related medicinal preparations.

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