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We established a quality evaluation method for Shuanghuanglian preparations based on an effect-constituent index (ECI), which is guided by the clinical efficacy of Shuanghuanglian and a dose-efficacy correlation. An HPLC method was used to establish the quantitative fingerprint of Shuanghuanglian from different manufacturers and to determine the content of 10 fingerprint components, including baicalin, chlorogenic acid, forsythin, galuteolin, wogonin, forsythoside A, luteolin, caffeic acid, baicalein, and scutellarin. Using Staphylococcus aureus as biological model, the potency of Shuanghuanglian preparations was determined by antibiotic microbial assay. Using the method of PLC-DA, the efficacious antibacterial components were screened by "dose-efficacy" correlation analysis. According to the antibacterial potency and content of the antibacterial ingredients, combined with the method of the custom weight coefficient, ECI was calculated and verified. The results show that the antibacterial ECI can facilitate evaluation of the efficacy of Shuanghuanglian based on the composition of its contents, providing a new method for the quality control of traditional Chinese medicine.
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Objective: To establish the HPLC fingerprint of the chemical components of the decoction of Radix Paeoniae Alba(RPA)and determine the content of paeoniflorin, so as to provide a scientific method for the quality char- acterization and control of RPA and establish a correlation between the quality of standard granules in classical prescrip- tion and the quality of RPA. Methods: Thermo Syncronis C18(250 mm×4.6 mm, 5 μm)chromatographic column was used, the mobile phase was constituted by acetonitrile(A)and 0.05 % phosphate aqueous solution(B), the detection wavelength was 230 nm, the column temperature was 30℃, the flow rate was 1.0 ml/min, and the injection volume was 20 μl;the gradient eluting procedure was 0-15 min, 5% A-15% A;15-45 min, 15% A-25% A;45-65 min, 25% A-50% A. Results: The HPLC fingerprint of RPA was established, 11 common peaks were identified by HPLC-Q-TOFMS/ MS, and the similarity of 10 batches were evaluated. The content determination of paeoniflorin in 10 batches of RPA decoction-lyophilized powders was also completed. Conclusion: This study provides a scientific and reliable method for the quality characterization and control of RPA as well as a reference for the quality characterization and control of the standard decoction and granules.
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In order to evaluate the quality of Styrax more comprehensively,this study attempted to establish an HPLC wavelength switching method to simultaneously determine the content of seven compounds in Styrax,and chemometrics were used to analyze the quality difference between different sources of Styrax,and finally establish a characteristic chromatogram of Styrax. The column was Agilent ZORBAX Extend C18( 4. 6 mm×250 mm,5 μm) with phase a mixture of acetonitrile-0. 1% phosphoric acid aqueous solution as the mobile phase in a gradient elution procedure; the detection wavelength was set as follows: 0-13. 5 min,194 nm( benzoic acid);13. 5-20. 5 min,278 nm( cinnamic acid); 20. 5-32 min,194 nm( benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid); 32-55 min,241 nm( abietic acid). The methodological verification results showed that when the injection masses of benzoic acid,cinnamic acid,benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid and abietic acid were0. 006 948-0. 694 8,0. 001 426-0. 142 6,0. 013 16-0. 658 0,0. 006 148-0. 614 8,0. 008 035-0. 803 5,0. 002 121-0. 212 1,and0. 010 172-1. 017 2 μg,respectively,there were good linear relationship between injection mass and peak area. The average recovery rates of seven compounds were in the range from 94. 34% to 105. 8%,and all RSD were less than 3. 0%( n = 6). The methodological verification results showed that the developed HPLC wavelength switching method has good accuracy and repeatability. The results of the sample analysis showed that the quality of Styrax from different sources was quite different. The chromatogram of Styrax reference material( S1) was used as the reference chromatogram to calculate the fingerprint similarity of each batch of samples. The results showed that the similarities of samples S2-S10 were 0. 952,0. 949,0. 981,0. 351,0. 751,0. 969,0. 979,0. 992 and 0. 971,respectively.The similarity values of other batches samples were satisfactory,except for sample S5 and S6,indicating that the quality difference among these samples is small. The similarity values of S11-S20 were 0. 060,0. 055,0. 054,0. 285,0. 092,0. 002,0. 044,0. 044,0. 044,and 0. 040,respectively. The results showed that compared with the sample S1,there was a large quality difference among S11-S20. Based on the chromatograms of S1-S10,the HPLC characteristic chromatograms of Styrax was established and the purpose is to give reference to other pharmaceutical researchers. The newly developed HPLC wavelength switching method have the advantages of simplicity,reproducibility and specificity,and the developed HPLC characteristic chromatograms provided a reference method for the overall quality evaluation of Styrax.
Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Phytochemicals , Quality Control , Reproducibility of Results , Styrax , ChemistryABSTRACT
This study was designed to establish a method to obtain the fingerprint chromatogram for the quantitative determination of Cordyceps sinensis in different sizes, a comparison of Cordyceps sinensis from five places was made to analyze its similarity and the content of main nucleosides (uridine, inoside, guanosine and adenosine). The assay was performed on a Waters XSelect HSS T3 C18 (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of water (A)-acetonitrile (B) at the flow rate of 0.6 mL·min-1 (0-5 min, 0 B; 5-15 min, 0→10% B; 15-30 min, 10%→20% B; 30-33 min, 20%→50% B; 33-35 min, 50%→0 B; 35-40 min, 0 B). The detection wavelength was 260 nm and the column temperature was set at 30℃, and the injection volume was 5 μL. The results showed that there was no significant difference of the nucleosides in samples from the same place of the different sizes, but contents of the nucleosides variate a lot by production places. More data are required for further research. The method is proved for scientific and specific formulation of the standard in evaluation of circulated Cordyceps sinensis.
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The biological potency assay and chemical fingerprint chromatogram were applied to quality evaluation of rhubarb. Using the biological potency as indicators, we evaluated the differences in quality of multiple batches of rhubarbs and related products. Using the platelet aggregation analyzer, we determined platelet aggregation rate in the different rhubarbs preparations, and calculated the biological potency based on the simplified probit principle. UPLC was adopted to establish the fingerprint spectra for rhubarbs. The spectral efficiency correlation analysis between chromatograms and biological potencies were conducted using the double variables of SPSS 22.0 software. We used three chemical composition to verify the potency. The biological potency results suggest that Rheum palmatum has a more potent activity than Rheum tanguticum, and wine-treated rhubarb had a higher potentcy than charred. We identified 10 elements in the Fingerprint Spectrum. The relevant elements including rhein-8-O-β-D-glucoside, emodin-8-O-β-D-glucoside and rhein have the strongest activity in the inhibition of platelet aggregation. In conclusion, this study provides a analytical method for rhubarb biological potency based on determination of the maximum antagonism rate model. The rhein may be the effective substance. It may serve as a reference in the quality control of wine processed rhubarb products.
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Objective To establish and compare HPLC fingerprint chromatograms of Dipsaci Radix decoction pieces, aqueous decoction and formula granules.Methods The HPLC analysis was carried out in Wondasil C18 column (4.6 mm × 250 mm, 5 μm) with a mobile phase of acetonitrile-0.1% phosphoric acid by gradient elution. The flow rate was 1.0 mL/min; the detection wavelength was set at 212 nm; the column temperature was kept at 30℃. Results The fingerprint chromatograms from 12 batches of Dipsaci Radix decoction pieces, aqueous decoction and formula granules were established respectively. 14 common peaks in the fingerprint chromatogram in the formula granules could be tracked in the aqueous decoction, and 13 common peaks in the fingerprint chromatogram could be tracked in the decoction pieces. 2 chemical compounds were identified, such as asperosaponinⅥ and chlorogenic acid.ConclusionThe method of HPLC fingerprint chromatograms is stable and with good repeatability. Dipsaci Radix decoction pieces, aqueous decoction and formula granules are basically the same chemical composition.
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OBJECTIVE:To establish the HPLC fingerprints for Herba clematidis in northeast. METHODS:HPLC was per-formed on the column of Hedera ODS-2 C18 with mobile phase of acetonitrile-0.5% phosphoric acid solution(gradient elution)at a flow rate of 1.0 mL/min,detection wavelength was 338 nm,column temperature was 30 ℃,and the injection volume was 20 μL. Using rutin as as a reference,the HPLC profiles of 10 batches of H. clematidis were determined,Similarity Evaluation Software for Chromatographic Fingerprint of Traditional Chinese Medicine(2004A edition) was used for the common peaks identification and similarity evaluation. RESULTS:There were 16 common peaks in the 10 batches of H. clematidis,similarity degree was higher than 0.9. It was proved that the HPLC profiles and control fingerprint profile of 10 batches of H. clematidis had good consistency. CONCLUSIONS:The established fingerprints can provide reference for the identification and quality evaluation of H. clematidis in northeast.
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Objective: To establish HPLC fingerprint chromatogram analysis for Mahuang Xuanfei Zhike syrup. Methods: The separation was performed on a Waters SunFire C18 column (250 mm × 4. 6 mm,5 μm), the mobile phase consisted of acetonitrile-0. 2% phosphoric acid with gradient elution at the flow rate of 1. 0 ml·min-1 , the detection wavelength was at 277 nm,the column temperature was at 30℃, and the sample size was 10 μl. Results: The precision, repeatability and stability of the fingerprint were measured. The fingerprints of 10 samples of Mahuang Xuanfei Zhike syrup revealed that there were twenty-four common peaks, and a-mong them, eight peaks were identified to Chinese, chlorogenic acid, caffeic acid, forsythin A, luteolin, apigenin, carotene and wild iris. Conclusion:The repeatability and information of chromatogram peaks of the method are satisfied, which provides a credible meth-od for controlling the quality of Mahuang Xuanfei Zhike syrup.
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Objective To study the correlation of fingerprint chromatograms of Cinnamomi Ramulus formula granules, decoction pieces and water decoction by HPLC; To investigate the difference of main chemical constituents among different forms. Methods The Diamonsil C18 column (4.6 mm × 250 mm, 5 μm) was used with mobile phase of acetonitrile and 0.1% phosphoric acid at the flow rate of 1.0 mL/min, with detection wave of 280 nm and temperature of 30 ℃. The detection of 10 batches of Cinnamomi Ramulus formula granules, 10 batches of decoction pieces and 10 batches of water decoction were established respectively. Results Totally 12 peaks in the HPLC fingerprint chromatogram from 10 batches of formula granules could be tracked in the water decoction; 10 peaks in the HPLC fingerprint chromatogram could be tracked in the decoction pieces. Three components, such as protocatechuic acid, coumarin and cinnamic acid were verified. Conclusion The main chemical components of Cinnamomi Ramulus formula granules and water decoction are basically the same, and the common component contents have similar proportion.
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This study is to establish the UPLC fingerprint of red ginseng. The separation was performed on a Waters Acquity BEH C₁₈ column (2.1 mm × 50 mm,1.7 μm), with the mobile phase consisting of acetonitrile and water for gradient elution. The detection wavelength was set at 203 nm. The UPLC fingerprint of red ginseng was established by using sample chromatography of 22 different purchase areas and 26 common peaks were found. Compared with the reference substances, 11 of the common peaks were identified as ginsenosides Rg₁, ginsenoside Re, ginsenoside Rf, ginsenoside Rh₁, ginsenoside Rg₂, ginsenoside Rb₁, 20(S)-ginsenoside F₁, ginsenoside Rb₂, ginsenoside Rb3, 20(S)-ginsenoside Rg₃ and 20(R)-ginsenoside Rg₃, respectively. It is worth noting that 20(S)-ginsenoside Rg₃ and 20(R)-ginsenoside Rg₃ are the characteristic ingredients of red ginseng, and they could be used not only for distinguishing red ginseng and ginseng, but also for process controlling of the preparation of red ginseng. The similarity was analyzed with' Similarity Evaluation System for Chromatographic Fingerprint of Chinese Materia Medica, and the similarity of 18 batches samples is up to 0.9. Compared to the literature methods, the method is simple, time-saving,specific for the separation of ginsenosides from red ginseng. So, this method could be used for the species identification and quality control of ginseng, red ginseng and American ginseng, and it will alsoprovide a theoretical basis of raising quality standards of the above mentioned Chinese herb medicines.
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OBJECTIVE: To establish the HPLC methods for determining the contents of the active ingredients and fingerprint chromatogram of Scutellaria barbata formula granules. METHOD: The HPLC analysis was carried out on a Wondasil C18 column (4.6 mm×250 mm, 5μm) with mobile phase consisting of methanol-acetonitrile-0.1% phosphoric acid (12.5:15:72.5) at the flow rate of 1.0 mL·min-1. The column temperature was maintained at 30t. The detection wavelength was set at 335 nm to determine the contents of scutellarin and scutellarein and 320 nm to establish the fingerprint chromatogram of Scutellaria barbata formula granules, medical materials, and aqueous decoction. RESULTS: The linear ranges of scutellarin and scutellarein were 0.074 0-0.518 0 μg and 0.051 6-0.3612 μg, respectively. The average recoveries were 103.18% and 99.99%, respectively. Nine peaks in the fingerprint chromatogram of formula granules could be tracked in the aqueous decoction, and eight peaks in the fingerprint chromatogram could be tracked in the medical materials. CONCLUSION: The methods can provide more information for the quality control of Scutellaria barbata formula granules.
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Objective To establish the chromatographic fingerprint of mushroom polysaccharides by 1-phenyl-3-methyl-5-pyrazolone( PMP) pre-column derivatization. Methods The mushroom polysaccharides was extracted by hot distilled water, precipitated by alcohol, and hydrolyzed into monosaccharides by Trifluoroacetic Acid (TFA). The hydrolysate was derivatized with 1-phenyl-3-methyl-5-pyrazolone ( PMP ) and tested via HPLC to study the monosaccharide components in mushroom polysaccharides. Results Fingerprint was established with 13 common peaks, 6 peaks in which were identified as mannose, D-glucuronic acid, D-glucose, galactose, xylose and L-fucose. The glucose accounted for the most, followed by mannose, galactose and fucose. Conclusion Development of fingerprint chromatogram by HPLC is a stable, simple, and repeatable way, which can be applied to the quality control of mushroom polysaccharides.
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OBJECTIVE:To establish the HPLC fingerprint chromatogram of Danzhen headache capsules. METHODS:HPLC method was adopted. The column was Dikma Diamonsil C18 with the mobile phase of methanol-acetonitrile-water(gradient elution) at the flow rate of 1.0 ml/min;the temperature was 40 ℃,the detection wavelength was 340 nm,the sample size was 20 μl and the detection time was 65 min. RESULTS:RSDs of precision,stability and reproducibility tests were no more than 0.23%;13 com-mon peaks were identified in 10 batches of Danzhen headache capsules and the similarity of all samples were higher than 0.90. CONCLUSIONS:The method is simple,accurate and reproducible,and can be used for the process stability evaluation and quali-ty control of Danzhen headache capsules.
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OBJECTIVE:To analysis the premier factor in formulating the fingerprint chromatography of Chinese medicinal materials METHODS:The fingerprint chromatograms of Chinese medicinal materials of different origins of breed variety and growth areas were compared RESULTS:There was obvious disparity in fingerprint chromatograms among Chinese medicinal materials of different origins of breed variety and growth areas CONCLUSION:Implementing GAP can ensure good quality of Chinese medicinal materials and is the key to formulate standard fingerprint chromatograms of Chinese medicinal materials
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Objective To establish the fingerprint chromatogram of Buzhong Yiqi Decoction(BYD) by multiple wavelength method,and to analyze the substance of formulas as a whole.Methods HPLC-PDA method was adopted.The chromatographic conditions were as follows:Hypersil ODS2 analytical column,the mobile phase consisting of 0.05 %phosphate acid and acetonitrile with gradient elution,detecting wavelength at 254 and 280 nm,the flow rate being 1.0 mL/min and the temperature of the column at 30 ℃.Results The methodological results were good.The results of dual-wavelength fingerprint chromatogram showed the all-around information of the fingerprints at 254 and 280 nm.The similarity of 10 batches of BuzhongYiqi Decoction was over 0.98.Conclusion Dual-wavelength fingerprint chromatogram can realize the analysis of a formulas as a whole,which supplies references for improving the quality control of BuzhongYiqi Decoction.
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AIM: To establish the fingerprint chromatogram of Hongjingtian Injection ( Rhodiola kirilowii (Regel.) Maxim. METHODS: HPLC with YWG C 18 column was used, the (a)MeOH ACN(1∶1)、(b) 0.07% H 3PO 4 H 2O gradient elution as a mobile phase and detection wavelength at 278nm . RESULTS: 17 peaks were indicated on the HPLC fingerprint of Hongjingtian Injection. The relative retention time and relative peak area were obtained with itself peak. CONCLUSION: The method is simple and accurate with good reproducibility and can be used as a quality control method of Hongjingtian Injection.
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Objective: To establish the fingerprint chromatogram of Tongguanteng Injection (caulis Marsdeniae Tenacissimae). Methods: HPLC with ZORBAX SB C 18 column was used, the (a) 0.05% H 3PO 4 H 2O and (b) ACN 0.05% H 3PO 4 H 2O (13∶87) (gradient elution) as a mobile phase and detection wavelength at 254nm. Results: 22 peaks were indicated on the HPLC fingerprint of Tongguanteng Injection. The relative retention time and relative peak area were obtained with itself peak at retention time 48.5 min. Conclusion: The method is simple and accurate with a good reproducibility and can be used as a quality control method for Tongguantent Injection.
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AIM: To establish a normal HPLC fingerprint chromatogram of herba Taraxaci in Henan Province. METHODS: 40 different kinds of herba Taraxaci were determined by RP-HPLC.Methanolthe solution of NaH_2PO_4(0.02 mol/L)(pH=3.8) gradient elution were adopted as a mobile phase,80 min the recording chromatogram chart and 1.0 mL/min of the velocity of flow detection wavelength was at 323 nm,column temperature was at 35℃. RESULTS: 9 steady mutual peaks were indicated. CONCLUSION: This method is simple,credible and of good reproducibility,can be used to identify and evaluate herba Taraxaci.
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AIM: To compare the fingerprints difference between total flavonoids and coumarins of Sarcandra glabra extract separated by macroporous adsorption resin. METHODS: To establish HPLC fingerprint chromatogram of Sarcandra glabra extract and to evaluate the constituents. RESULTS: The difference fingerprint was showed in total flavonoid part and coumarin part. CONCLUSION: Drug action part could be separated by macroporous adsorption resin and exosyndromed by Spectrogram fingerprints.
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AIM: To provide a basis for appraising quality standard of Baohe Pill (Fructus Gataegi, Massa medicata fermentata, Rhizoma pinelliae, Pericapium citr reticulatae, Fructus forsythiae, Semen raphani, Fructus Mordei germinatus, Poria) inclusive of its RP-HPLC fingerprint chromatogram. METHODS: The chromatographic column was Kromasil C_ 18 column (4.6 mm?250 mm, i.d, 5-?m particle size). The mobile phase was 0.5% solution of ammonium dihydrogen phosphate (NH_4H_2PO_4), and the flow rate was 0.8 mL/min with UV detector at 214 nm. RESULTS: The RP-HPLC fingerprint chromatogram of Baohe Pill was established. In the experiment, for precision and repeatability, the RSD of each area of common peak was less than 3%. CONCLUSION: This method is simple and reliable.