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OBJECTIVE： To establish a method for simultaneous determination of 7 kinds of anti-rheumatic active ingredients in Mongolian medicine Sendeng-4 decoction powder， such as catechin， jasminoidin， dihydromyricetin， texifolin， rutin， myricetin and quercetin. METHODS： HPLC-DAD method was adopted. The determination was performed on Sil Green C18 column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid solution （gradient elution） at the flow rate of 1 mL/min. The detection wavelength was set at 238 nm， and column temperature was 30 ℃. The sample size was 10 μL. RESULTS： The linear range of catechin， jasminoidin， dihydromyricetin， texifolin， rutin， myricetin and quercetin were 8.590-2 290， 10.56-3 901， 13.00-3 958， 8.815-564.2， 4.030-257.8， 8.130-750.5， 7.075-454.2 μg/mL （r≥0.999 1）， respectively； the limits of detection were 0.429 5， 0.264 0， 0.325 0， 0.220 4， 0.201 5， 0.203 2， 0.176 9 μg/mL， respectively； the limits of quantification were 1.030， 1.321， 1.302， 1.397， 1.637， 0.813 0， 0.707 5 μg/mL， respectively. RSDs of precision， stability （48 h） and repetition tests were all lower than 2.0％ （n＝6）. The average recoveries were 96.24％-99.28％ （RSD＝1.03％-1.63％， n＝6）. CONCLUSIONS： The established method is simple， accurate and reproducible， and can be used for simultaneous determination of catechin， jasminoidin， dihydromyricetin， texifolin， rutin， myricetin and quercetin in Mongolian medicine Sendeng-4 decoction powder.
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Objective To study the protein binding rates ofgardenioside,paeoniflorin and naringin in Weiyanling granules in bovine serum albumin,rat plasma and human plasma.Methods The equilibrium dialysis method was carried to determine the binding-rates of three components in Weiyanling granules in bovine serum albumin,rat plasma and human plasma.The HPLC method was used to determine the mass concentration of three components in weiyanling granules in inner and outer dialysis and to calculate the plasma protein-binding rates.Results The linear relationship,precision,extraction recovery and stability of gardenoside,paeoniflorin and naringin all conformed to the methodological requirements.Within the low,middle and high concentration (5.084,10.04 and 20.08 g/L) of Weiyanling granules,the protein-binding rates of gardenioside and bovine serum albumin were 23.77％ ± 13.39％,10.75％ ± 1.34％,5.82％ ± 6.53％,respectively;the protein-binding rates of paeoniflorin were 51.81％ ± 6.53％,30.12％ ± 6.61％,21.39％ ± 9.45％,respectively;the protein-binding rates of naringin were 70.21％ ± 3.31％,67.61％ ± 1.31％,56.00％ ± 3.46％,respectively;the protein-binding rates of gardenioside and rat plasma were 71.56％ ± 3.00 ％,43.56％ ± 12.22％,40.63％ ± 4.73％,respectively;the protein-binding rates ofpaeoniflorin and rat plasma were 55.72％ ± 1.60％,47.59％ ± 6.33％,40.07％ ± 0.72％,respectively;the protein-binding rates of naringin and rat plasma were 85.85％ ± 3.53％,85.38％ ± 0.99％,79.99％ ± 2.57％,respectively;the protein-binding rates of gardenioside and human plasma were 13.56％ ± 2.40％,3.02％ ± 2.41％,5.82％ ± 2.08％,respectively;the protein-binding rates of paeoniflorin and human plasma were 9.49％ ± 5.23％,5.01％ ± 1.10％,3.98％ ± 1.54％,respectively;the protein-binding rates of naringin and human plasma were 25.04％ ± 2.61％,26.09％ ± 13.82％,20.20％ ± 2.24％,respectively.Conclusions Within 5.084,10.04 and 20.08 g/L,the protein binding-rate of gardenioside,paeoniflorin and naringin were shown asfollow,rat plasma ＞bovine serum albumin ＞ human plasma.There were significant differences in species.
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Objective To optimize a method for extracting traditional Chinese medicine composition with insomnia,and to prepare the insomnia granules for quality control.Methods The optimal extraction process was screened by orthogonal test using high-performance liquid chromatography with geniposide as the evaluation index.The particle size,bulk density,angle of repose,moisture,solubility,hygroscopicity and loading difference of the insomnia granule were evaluated,and the difference between the trial test and the pilot test were analyzed to comprehensively monitor the quality of the insomnia granule.Results The best extraction process was to add 10 times of water and cooked it three times for 1.5 hours each time.The average yield rate of dry extract of the pilot test and trial test was 22.10％,15.52％,and the average yield of powder was 84.96％ and 93.12％,respectively.The conversion rate from the pilot test to the trial test is 76.97％.Both the trial test and the pilot test particles met the quality requirements of the 2015 edition of the pharmacopoeia.Conclusions The preparation method of the insomnia granules is simple and the quality is uniform.The results of the pilot scale showed that the conversion rate is high,the quality is controllable,and the technical feasibility of industrial production is obtained.
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Objective: To establish a quantitative analysis of multi-components with a single-marker (QAMS) method for the determination of the nine components in Reduning Injection (RI), comparing with the external standard method, and to evaluate the adaptation and application of QAMS method in the quality control of RI. Methods: Chlorogenic acid, isochlorogenic acid A, and gardenoside were used as the internal reference substances. The relative correlation factors (f) of neochlorogenic acid, cryptochlorogenic acid, and caffeic acid to chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C to isochlorogenic acid A, and secoxyloganin to gardenoside were calculated and established. The results were compared with those obtained by the external standard method. Results: Within the linear ranges, the f values of chlorogenic acid to neochlorogenic acid, cryptochlorogenic acid, and caffeic acid were 0.965, 0.991, and 0.555, respectively; isochlorogenic acid A to isochlorogenic acid B and isochlorogenic acid C were 1.283 and 1.129, respectively; jasminoidin to secoxyloganin was 1.030. The two methods did not show the significant difference in assay results. Conclusion: The QAMS method is feasible and credible, and could be used to determine the multiple components in RI.
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AIM: To establish a method for determining baicalin, jasminoidin, cholalic acid and hyodeoxycholic acid in Qingkailing Granules(chololic acid, hyodeoxycholic acid, baicalin, Fructus Gardeniae, Cornu Bubali, Flos Longicerae Japonicae, Radix lsatidis, Concha Margaritifera). METHODS: Part 1 (determination of baicalin and jasminoidin):The HPLC method was carried out on kromasil~(TM)C_(18) column(4.6 mm×150 mm,5 μm) with acetonitrile-water(10: 90)as mobile phase, gradient elution; the UV detection wavelength was at 238 nm. Part 2 (determination of cholalic acid and hyodeoxycholic acid):The HPLC method was carried out on kromasil~(TM)C_(18) column(4.6 mm×150 mm,5 μm) with acetonitrile-water-phosphonic acid(35:65:0.1) as mobile phase,gradient elution;the UV detection wavelength was at 192 nm. RESULTS: The average recoveries were 99.30% with RSD of 0.2% for baicalin; 99.50% with RSD of 0.4% for jasminoidin; 99.04% with RSD of 0.2% for hyodeoxycholic acid; 99.06% with RSD of 0.4% for cholalic acid; respectively. CONCLUSION: The assay demonstrats that the method is simple,it has the adequate accuracy and selectivity to quantify the four active components in Qingkailing Granules.
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Objective:To establish the quality standard for Qixue Bawei Granule.Methods:Calculus Bovis and Radix Arnebiae were identified by TLC.Jasminoidin was determined by a HPLC method.Results:TLC spots were clear and specific.A good linear relationship between peak area and concentration of Jasminoidin was found at the range of 0.128-0.640?g with a correlation coefficient (r=0.9999).The average recovery of Jasminoidin was 99.02% as RSD 1.8 %(n=5).Conclusion:The methods were reliable,accurate and specific.It may be used to the quality control of the preparation.
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OBJECTIVE:To establish an HPLC method for the determination of the contents of baicalin,berberine hydrochloride and jasminoidin in Coptidis decoction for detoxification.METHODS:The samples were separated on Shimazu Sim-pack VP-ODS C18(250 mm?4.6 mm,5 ?m)with mobile phase consisted of acetonitrile-(0.05% potassium dihydrogen phosphate+0.05% trolamine solution,with pH adjusted to 3.0 by phosphoric acid)in gradient elution under a detection wavelength of 254 nm.RESULTS:The linear ranges of jasminoidin,berberine hydrochloride and baicalin were 0.4～2.0 mg?mL-1(r=0.998 1),0.020～0.40 mg?mL-1(r=0.992 0)and 0.020～0.40 mg?mL-1(r=0.996 3),respectively,and their average recoveries were 99.8%,97.5% and 98.1%,respectively,with RSD at 1.8%,2.5% and 1.5%,respectively(n=6 for all the three).CONCLUSION:The established method is specific,sensitive,simple and applicable for the quality control of Coptidis decoction for detoxification.
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OBJECTIVE:To prepare Sanzi capsules and establish the Standard of its quality.METHODS:Water decocting method was applied to extract physic liquor,thin-layer chromatography(TLC)was used for qualitative identification,and high efficiency liquid chromatography(HPLC)was used to determine the content of Jasminoidin in the preparation.RESULTS:Feature spots of Fructus Gardeniae,Fructus Chebulae,Fructus Toosendan were identified by TLC,with no sensible interference seen in the negative control.The linear range for Jasminoidin was 3.0～ 30? g? mL-1(r=0.999 9)with average recovery rate at 100.06%(RSD=1.17%).CONCLUSION:The preparation method is well-grounded,highly-specific and reproducible in property identification,accurate and reliable in content determination,and can be used for the quality control of Sanzi capsules.
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OBEJETIVE:To determinate simultaneously the contents of berberine hydrochloride,palmatine hydrochloride,jatrorrhizine hydrochloride,baicalin and jasminoidin in coptis chinensis detoxication capsule by HPLC.METHODS:3different UV wavelengths were adopted simultaneous in the determination in which Diamonsil C 18 was taken as the chromatographic column and water-methanol-0.05%H 3 PO 4 (gradient elution)was taken as mobile phase,the column temperature was set at35℃and the flow rate was1.0ml/min,the detection wavelength were345nm,280nm and238nm respectively and the sample size was10?l.RESULTS:They took good linear relationships when the respective sample size of berberine hydrochloride,pal-matine hydrochloride,jatrorrhizine hydrochloride,baicalin and jasminoidin were at0.105?g～1.680?g(r=0.9999),0.045?g～ 0.720?g(r=0.9998),0.065?g～1.040?g(r=0.9997),0.190?g～3.040?g(r=0.9999)and0.145?g～2.320?g(r=0.9999);Their respective average recovery rates were99.11%,98.19%,97.21%,98.52%and99.22%.CONCLUSION:This method is fast,reproducible,sensitive,and which can provide a more reasonable and reliable quality control for coptis chinensis detoxi-cation capsule.
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OBJECTIVE:To establish a RP-HPLC method for determination of Jasminoidin in Yinxie tablets.METHO_ DS:The HPLC system consisted of C 18 column(250mm?4.6mm,5?m),0.01%phosphoric acid-acetonitrile(87∶13)mixture as a mobile phase,detection wavelength at238nm and1.0ml/min of flow rate.RESULTS:The calibration curve of Jasminoidin was linear in the concentration range of20～200?g/ml(r=0.9995),RSD=0.98%(n=5).The average recovery was101.8%(RSD=0.54%).CONCLUSION:This method is simple,quick and specific,and suitable for the quality control of this prepa?ration.
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【Objective】To observe the effect of different active ingredients from Chinese herbal medicine on interleukin 8(IL-8) secretion and Toll-like receptor 4(TLR4) mRNA expression in human intestinal tumor cell(HT-29)line.【Methods】Reverse transcription polymerase chain reaction(RT-PCR) was used to detect TLR4 mRNA expression,and enzyme-linked immunosorbent assay(ELISA) was used to examine IL-8 secretion.【Results】Astragaloside and emodin inhibited TLR4 mRNA expression stimulated by interferon ?(IFN-?),and emodin decreased IL-8 secretion stimulated by IFN-? and lipopolysaccharide(LPS).However,curcumin,naringin and jasminoidin had no effect on TLR4 mRNA expression.【Conclusion】The anti-inflammatory cellular mechanism of emodin may be related to the inhibition of TLR4 mRNA expression stimulated by IFN-?,and to the inhibition of IL-8 secretion stimulated by IFN? and LPS in HT-29 cell line.
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Objective To study the collision-induced dissociation fragmentation pathways of the jasminoidin and catalpol in ESI-Msn. Methods The samples were studied by using high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-Msn) both in positive and negative. Results The collision-induced dissociation fragmentation pathways of both compounds were described. In the spectrum of two compounds, the loss of glucose residue and whole glucose were observed in positive mode, while only the loss of glucose residue could be observed in negative mode. Furthermore, we found that as the effect of the substituting groups, the fragment ions of jasminoidin were more in positive mode and those of catalpol were more in negative mode. Conclusion Conclusion The established method could be used for the sensitive and rapid identification of this kind of iridoid glycosides。
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AIM: To establish a HPLC quality control for Chizhihuang Capsules(Radix Paeoniae Rubra, Fructus Gardeniae, Radix et Rhizoma Rhei, etc.). METHODS: Shim pack C 18 column was used, and jasminoidin and paeoniflorin were determined at the same time and detection wavelength at 230nm. RESULTS: The standard curve of jasminoidin was linear in the range of 0.30～1.50?g. The average recovery and RSD were 99.58 and 1.57% ( n =5), respectively. The standard curve of paeoniflorin was linear in the range of 0.26～ 1.30?g . The average recovery and RSD were 99.11 and 1.29% ( n =5), respectively. CONCLUSIONS: This method is a convenient, reliable and accurate for the quality control of Chizhihuang Capsules.
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AIM: To establish a method for determining baicalin,jasminoidin,cholalic acid and hyodeoxycho-lic acid in Qingkailing Granules(chololic acid,hyodeoxycholic acid,baicalin,Fructus Gardeniae,Cornu Bubali, Flos Longicerae Japonicae,Radix Isatidis,Concha Margaritifera). METHODS: Part 1(determination of baicalin and jasminoidin):The HPLC method was carried out on kromasilTMC_18 column(4.6 mm?150 mm,5 ?m) with acetonitrile-water(10∶90)as mobile phase,gradient elution;the UV detection wavelength was at 238 nm.Part 2(determination of cholalic acid and hyodeoxycholic acid):The HPLC method was carried out on kromasilTMC_18 column(4.6 mm?150 mm,5 ?m) with acetonitrile-water-phosphonic acid(35∶65∶0.1) as mobile phase,gradient elution;the UV detection wavelength was at 192 nm. RESULTS: The average recoveries were 99.30% with RSD of 0.2% for baicalin;99.50% with RSD of 0.4% for jasminoidin;99.04% with RSD of 0.2% for hyodeoxycholic acid;99.06% with RSD of 0.4% for cholalic acid;respectively.CONCLUSION: The assay demonstrats that the method is simple,it has the adequate accuracy and selectivity to quantify the four active components in Qingkailing Granules.
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AIM:To determine gentianaceae and jasminoidin in Longhui Capsules (Radix et Rhizoma Gentia-nae, Aloe, Fructus Gardeniae, etc.) METHODS: The Waters Symmetry C_ 18 column (4.6 mm?150 mm, 5 ?m) was used with mobile phase of methanol-water (17∶83). The flow rate was 1.0 mL/min. The detecting wavelength was at 254 nm, and the column temperature was at 30 ℃. RESULTS: The methodological study showed that a good linear correlation existed in the range of 60.72-454.4 ng for gentianaceae and the range of 96.32 -722.40 ng for jasminoidin. The average recovery of gentianaceae was 99.57%(n=9) and RSD was 1.27% , jasminoidin was 99.10%(n=9) and RSD was 2.30%. CONCLUSION: The method is simple, accurate and can be used for quality control of the preparation.
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OBJECTIVE:To investigate the equivalence of preparations of traditional Chinese medicines with decoction and pill as the representative dosage forms so as to lay a foundation for the evaluation of equivalence.METHODS:Taking the contents of gentiopicroside and geniposide and water soluble extractive as indexes to investigate the equivalence between decoction for Longdan xiegan tang and Longdan xiegan pills.RESULTS:Evaluated by the indexes of contents of gentiopicroside and geniposide,the current daily oral dosage of the decoction was 6.39 times superior to the pill;taking water soluble extractive as index,the decoction was 4.02 times superior to the pill.CONCLUSION:To be equivalent to the decoction,the current daily oral dosage of the pill should be increased appropriately.The degree of increase should be based on the final results of pharmacological and clinical studies.
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OBJECTIVE:To establish a RP-HPLC method for the determination of baicalin and jasminoidin in Qingkailing Injection.METHODS:It was performed on DiamonsilTM C18 column with acetonitrile-20 mmol?L-1 sodium dihydrogen phosphate solution (20:80)as mobile phase.The flow rate was 1.0 mL?min-1.The detection wavelength was 238 nm.RESULTS:The liner range of baicalin was 1～50?g?mL-1,(r=0.999 5)and the average recovery was 100.75%(RSD=1.75%);The liner range of jasminoidin was 0.1～10?g?mL-1(r=0.999 7)and the average recovery was 100.63%(RSD=1.35%).CONCLUSION:This method is rapid,simple,accurate and sensitive.It can be used for quality control of Qingkailing Injection.
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Objective:To establish a method for the determination of jasminoidin and paeoniflorin in Qiyitang Granules.Methods:The analytical column was a Agilent Eclipse XDB-C18 column(4.5?150mm,5?m).The mobile phase consisted of acetonitrile-0.1%H3PO4(12:88,V/V),flow rate was 1.0ml/min.The detection wavelength was 230 nm.Rusults:Jasminoidin and paeoniflorin were separated utterly and the linear correlation was good. The average recoveries of high,middle and low concentration of jasminoidin were 106.2%,97.5% and 98.1% respectively with RSD of 0.96%,1.23% and 1.62%(n=3)respectively.The average recoveries from paeoniflorin were 101.3%,99.5% and 98.2% respectively with RSD being 1.19%,1.33% and 1.58%(n=3),respectively. Conclusions:The method is simple,reproducible,accurate and reliable.It may be used for the quality control of this granules.