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Objective:To compare the total daily doses of 16 active components in big honeyed pills, concentrated pills and tablets of Fuzi Lizhongwan. Method:Three dosage forms of Fuzi Lizhongwan were prepared according to the process described in the literature. RRLC-QqQ-MS was employed to analyze the contents of 16 active ingredients with mobile phase of 0.1%formic acid aqueous solution-0.1%formic acid acetonitrile solution for gradient elution,the separation was performed on a Accucore RP-MS column(2.1 mm×100 mm, 2.6 μm) with a flow rate of 0.3 mL·min-1 and the column temperature at 30℃, the mass spectrometry condition was electrospray ion source, positive and negative ion switching mode for detection, multi-reaction monitoring mode(MRM) for scanning. The contents of 16 active ingredients were calculated, and the normalization arithmetic method was used for comparing the total daily doses of these active ingredients in three dosage forms of Fuzi Lizhongwan. Result:Processed products of Aconiti Lateralis Radix Praeparata were used as raw powder in preparation process of the three dosage forms, so there was no significant difference in the contents of six alkaloids in the three dosage forms, while the contents of other 10 active ingredients from Zingiberis Rhizoma, Codonopsis Radix, Atractylodis Macrocephalae Rhizoma and Glycyrrhizae Radix et Rhizoma Praeparata cum Melle were significantly higher in big honeyed pills than those in concentrated pills or tablets(PConclusion:The total daily doses of 16 active ingredients in the three dosage forms of Fuzi Lizhongwan are significantly different caused by preparation process, prescription and dosage.
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Objective:To optimize the forming technology of Zuojin concentrated pills. Methods: Single factor test was used to optimize the types of excipients and wetting agents with the shaping result as the index. Orthogonal test was used to optimize the forming technology taking the dissolution time,shaping rate and appearance quality as the evaluation indices,and the proportion of excipients, the rate of drugs to excipients and wetting agent amount as the investigation factors. Results: The best forming technology of Zuojin concentrated pills was as follows:MCC and PVP-K30 were used as the excipients with the ratio of 3:1,the ratio of drugs to excipients was 1:1,5% water was used as the wetting agent to obtain the damp mass,and then Zuojin concentrated pills were prepared in a pill machine. Conclusion:The optimized forming technology is stable with good reproducibility,and the pills are round and smooth with u-niform color,whose quality meets the requirements described in Chinese Pharmacopoeia(2015 edition,partⅣ,page 0108 for concen-trated pills). The study provides reference for the further study.
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OBJECTIVE:To establish the HPLC fingerprint of Zhibai dihuang pills(concentrated pills),and to evaluate its quality. METHODS:The determination was performed on Dikma Diamonsil C18column with mobile phase consisted of 0.1%acetic acid solution-methanol(gradient elution)at the flow rate of 1.0 mL/min. The detection wavelength was set at 260 nm,and column temperature was 30 ℃. The sample size was 10 μL. Using paeonol as reference,HPLC chromatograms of samples from A, B,C manufacturers within validity period and samples from manufacturer A within validity period and out of validity period were drawn. The similarity of HPLC chromatogram for samples from A,B and C manufacturers and samples from A manufacturer within validity period and out of validity period was evaluated by TCM Chromatogram Fingerprint Similarity Evaluation System (2004 A). Common peaks of HPLC chromatogram for 3 manufacturers sample within validity period were confirmed. RESULTS:There were 24,29 and 32 common peaks in HPLC chromatograms for each 10 batches of samples from manufacturer A,B and C within validity period,respectively. The similarity of corresponding HPLC chromatograms of samples from manufacturer A,B and C compared with control HPLC chromatography were all higher than 0.94 with good agreement. HPLC chromatograms of sample from A manufacturer within validity period had good agreement with that from A manufacturer out of validity period. CONCLUSIONS:Established HPLC fingerprint analysis method can represent the quality of Zhibai dihuang pills (concentrated pills),but cannot effectively identify the expired samples.
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AIM To evaluate the stability of Zuogui Concentrated Pills.METHODS HPLC was applied to determining the contents of acteoside,loganin and hyperoside,whose relative contents were detected by classical constant temperature accelerated test,after which the fitting of kinetic equation was conducted.The period of validity was predicted by classical constant temperature method and multivariate linear model,and the stability was investigated by high temperature,high humidity,strong light,accelerated and long-term tests.RESULTS The degradation of acteoside,loganin and hyperoside accorded with the first-order kinetic process.The periods of validity were found to be 25.6 months and 23.9 months by two methods,respectively.No obvious changes were observed on three constituents' contents,appearance and character,disintegration time limit,moisture content and weight variation under various tests.CONCLUSION A tentatively scheduled two-year validity period is suitable for Zuogui Concentrated Pills due to its good stability.
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Objective:To optimize the extraction parameters for the water extract of Tangganjian concentrated pills .Methods:U-sing the content of paeoniflorin and extraction yield as the evaluation indices .An HPLC was used to determine the content of peoniflorin in the extract, and the chromatographic conditions were as follows: a WondaSil C18 chromatographic column (250 mm ×4.6 mm, 5μm), the mobile phase was acetonitrile-0.1%phosphoric acid solution (16∶84) with a flow rate of 1 ml· min-1, the column tem-perature was 30℃and the detection wavelength was 230 nm.The amount of water , extraction time and extraction times were regarded as the influencing factors ,an orthogonal design was adopted to develop the analysis of variance for extraction parameters for water ex -tract.Results:The optimal extraction process was as follows:adding 12-fold amount of water and extracting 3 times with 1 h for each time.Conclusion:The optimum extraction process is reasonable , stable and feasible, which provides experimental basis for the extrac-tion process of Tangganjian concentrated pills .
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Objective: To establish a determination method for the simultaneous determination of the multiple components in Liuwei Dihuang Concentrated Pills (LDCP). Methods: The contents of gallic acid, 5-hydroxymethyl furfural, morroniside, loganin, paeoniflorin, paeonol, and ursolic acid were used as observing indexes. HPLC method, Agilent TC-C18 (250 mm × 4.6 mm, 5 μm) column using acetonitrile-0.02% TFA as mobile phase, gradient elution volume flow was 1.0 mL/min, column temperature was 30℃; Detection wavelengths were 0-60 min, 238 nm, 60-70 min, and 210 nm; Cluster analysis method was used to compare the differences of LDCP among 20 different manufacturers. Results: The seven ingredients in LDCP from different manufacturers were determined. There was difference among them, the contents of paeoniflorin showed appreciable difference. The products from 20 manufacturers were divided into two categories by the cluster analysis, and showed obvious difference between them. The numbers 4, 6, 8, 9, 11, 14 and 16 were classified into one group, which quality difference was relatively minor; The products from other manufacturers belonged to one category and there were little differences among the seven components. Conclusion: The methodology research shows that this methed could fit the demand of determination and provides some guidance to advance the quality evaluation of LDCP.
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Objective:To study the qualitative and quantitative methods of Shenbai concentrated pills. Methods:Danshen root and lightyellow sophora root in Shenbai concentrated pills were identified with the method of TLC. The contents of astragaloside Ⅳ and paeoniflorin were determined with the method of HPLC. Results: For TLC, the spots of the two herbal drugs were well separated and without interference. Quantitative analysis of HPLC showed that the average recovery of astragaloside 1V was 100.82% (RSD1.73%) with the RSD values of precision, repeatability and stability tests were 2.79%, 1.48% and 1.44%, respectively; and the average recovery of paeoniflorin was 99.83% (RSD2.34%) with the RSD values of precision, repeataibility and stability tests were 2.25%, 2.16% and 1.60%, respectively. Conclusions: The methods set up by this study are accurate and easy to perform with the merits of good resolution, specificity and reproducibility. It could effectively control the quality of Shenbai concentrated pills.
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Objective To set up the quality standard of Shenbai concentrated pills. Methods Radix Astragali, Radix Paeoniae Rubra and Rhizoma Imperatea in Shenbai concentrated pills were identified with the method of TLC. The concentration of salvianolic acid B was determined with the method of HPLC. Results For TLC, the chromatogram spots of Radix Astragali, Radix Paeoniae Rubra and Rhizoma Imperatea were well separated and without interference in their negative controls. Quantitative analysis of HPLC showed that the average recovery of salvianolic acid B was 99.74% (RSD=2.08%) with the RSD of precision, reproducibility and stability was 1.74%, 1.19% and 1.70%, respectively. Conclusions The methods set up by this study are easy, accurate and stable, and can be used as the quality control standard of Shenbai concentrated pills.
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Objective To optimize the extraction technique for Modified Danggui Buxue Concentrated Pills.Methods The extraction technique was studied by orthogonal design with the yield of astragaloside Ⅳ and total polysaccharides as the investigative indexes.Results The optimal extraction technique is as follows: adding 8-fold water,decocting 3 times and lasting 70 minutes for each time.Conclusion The optimized extraction technique is simple,reasonable and stable,which supplies experimental evidence for the further development of Modified Danggui Buxue Concentrated Pills.
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AIM: To establish the method for quality control of Guipi Pills(concentrated pill) (Radix Codonopsis,Rhizoma Atractylodis macrocephalae,Radix Astragali,Radix et Rhizoma Glycyrrhizae,etc).and a quantitative method of determining astragaloside IV. METHODS: Radix Codonopsis,Radix Angelicae Sinensis,Radix et Rhizoma Glycyrrhizae and Radix Aucklandiae in the pill were identified by TLC.Astragaloside IV in the pill was determined by HPLC-ELSD. RESULTS: For astragaloside IV,the linear range was within 25.4-508.3 ?g and the average recovery was 99.1%,r=0.999 7 with RSD of 0.8%. CONCLUSION: The method is simple,reliable,accurate,practical.It can be used in the quality control of Gui Pipills(concentrated pills).
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OBJECTIVE:To determine Sarsasapogenin in Jujube seed concentrated pills by RP-HPLC-ELSD.METHODS:Separation of Sarsasapogenin was performed on Zorbax C18 column with methanol-water (90:10)as a mobile phase at a flow rate of 1.0mL?min-1.The temperature of the drift tube was 85℃and the air flow-rate was at 1.71mL?min-1.RESULTS:The linear range of Sarsasapogenin was 0.112 7～0.676 2mg?mL-1(r=0.998 3).The average recovery was 99.83%(RSD=0.93%).CONCLUSION:The method is simple,accurate and reproducible,and suitable for the quality control of Jujube seed concentrated pills.