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Objective To investigate the effects of the three methods of decocting with deslag, decocting without deslag, and double decocting on the content of nine ingredients baicalin, baicalein, ginsenoside Re, ginsenoside Rb1, monoammonium glycyrrhizinate hydrate, liquiritin, 6-gingerol, berberine hydrochloride, palmatine hydrochloride, and total flavonoids in Banxia Xiexin Decoction (BXD). Methods Nine index components were determined by HPLC. The HPLC analysis was performed on Welch Ultimate XB-C18 column (250 mm × 4.6 mm, 5 μm) with mobile phase of acetonitrile-0.1% phosphate aqueous solution for gradient elution; And carried out at column temperature of 28 ℃, volume flow of 0.9 mL/min, and detection wavelength of 203, 252, 280, and 355 nm. The total flavonoids were determined by colorimetry. Results Nine kinds of ingredients and total flavonoids could be detected in three different decoctions. In the method of decocting with deslag, baicalin, baicalein, ginsenoside Rb1, monoammonium glycyrrhizinate hydrate, and liquiritin increased by 10.01%, 12.88%, 29.09%, 16.75%, and 15.02%, respectively, compared with decocting without deslag; It decreased by 5.54%, 4.15%, 14.49%, 7.85%, and 9.18%, respectively compared with double decocting; Ginsenoside Re, 6-gingerol, berberine hydrochloride, and palmatine hydrochloride increased by 37.90%, 3.78%, 5.33%, and 5.99% compared with decocting without deslag, respectively; compared to the double decocting methods, it increased by 1.07%, 11.57%, 3.41%, and 1.93%. The total flavonoids increased 22.61% higher than decocting without deslag and 6.54% higher than double decocting. Conclusion: The results can effectively reflect the quality difference of different decocting methods. Among the three methods of decoction, the method of decocting without deslag has significantly improved the dissolution of the active ingredients of each component in the decoction, and improve the clinical efficacy of BXD to a certain extent. It provides a good experimental basis for the decocting without deslag method used in Zhang Zhongjing’s Treatise on Febrile Diseases.
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OBJECTIVE:To establish a method for simultaneous determination of 3 components in Li'ermian capsule,including berberine hydrochloride,palmatine hydrochloride and cinnamaldehyde.METHODS:HPLC method was adopted.The determination was performed on Agilent Zorbax SB-C18 with mobile phase consisted of acetonitrile-0.05 mol/L potassium dihydrogen phosphate solution (23 ∶ 77,V/V) at the flow rate of 1.0 mL/min.The detection wavelengths were set at 345 nm (0-20 min,berberine hydrochloride,palmatine hydrochloride) and 290 nm (＞20-30 min,cinnamaldehyde),and column temperature was 30 ℃.The sample size was 10 μL.RESULTS:The linear ranges of berberine hydrochloride,palmatine hydrochloride and cinnamaldehyde were 0.036 80-0.736 0,0.016 76-0.335 2,0.004 140-0.082 80 μg (r≥0.999 5).The limits of detection were 0.110 4,0.050 3,0.124 2 ng,and the limits of quantitation were 0.368 0,0.167 6,0.414 0 ng,respectively.RSDs of precision,stability (12 h) and reproducibility tests were all lower than 2.0％ (n=6).The recoveries were 96.16％-99.73％ (RSD=0.99％-1.21％,n=6).CONCLUSIONS:Established method is simple,reproducible and suitable for simultaneous determination of 3 components such as berberine hydrochloride in Li'ermian capsule.
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OBJECTIVE:To establish a method for simultaneous determination of gallic acid,magnoflorine,ellagic acid,jatrorrhizine hydrochloride,palmatine hydrochloride,berberine hydrochloride and curcumin in Siwei jianghuang decoction powder.METHODS:HPLC method was adopted.The determination was performed on Capcell Pak C18-MG Ⅱ column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid (gradient elution) at the flow rate of 0.8 mL/min.The detection wavelengths were 270 nm (0-60 min,gallic acid,magnoflorine,ellagic acid,jatrorrhizine hydrochloride,palmatine hydrochloride,berberine hydrochloride) and 428 nm (60-70 min,curcumin).The column temperature was set at 30 ℃,and sample size was 10 μL.RESULTS:The linear ranges of gallic acid,magnoflorine,ellagic acid,jatrorrhizine hydrochloride,palmatine hydrochloride,berberine hydrochloride and curcumin were 0.249 6-1.497 6,0.284 0-1.704 0,0.075 6-0.453 6,0.015 9-0.095 9,0.023 6-0.141 6,0.098 2-0.589 0 and 0.060 4-0.362 4 μtg (r≥0.999 8).The limits of detection were 6.24,4.73,7.56,2.36,3.20,6.54,6.04 ng,and the limits of quantitation were 17.47,16.08,20.86,7.31,10.24,19.62,19.32 ng,respectively.RSDs of precision,stability (12 h),reproducibility tests were lower than 2.0％ (n=6).The recoveries were 95.45％-103.47％ (RSD=0.86％-1.98％,n=9).CONCLUSIONS:Established method is simple,accurate,reliable and suitable for simultaneous determination of 7 components such as gallic acid in Siwei jianghuang decoction powder.
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AIM To develop an HPLC method for the simultaneous content determination of berberine hydrochloride,jatrorrhizine hydrochloride,palmatine hydrochloride,kaempferol,luteolin and apigenin in Qingre Zhili Pills (Berberidis Radix and Portulacae Herba).METHODS The analysis of methanol extract of this drug was performed on a 35 ℃ thermostatic Agilent TC-C18 column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.02％ potassium dihydrogen phosphate flowing at 0.9 mL/min in a gradient elution manner,and the detection wavelengths were set at 265 nm and 360 nm.RESULTS Six constituents showed good linear relationships within their own ranges (r≥0.999 3),whose average recoveries were 97.16％-99.90％ with the RSDs of 0.62％-1.48％.CONCLUSION This simple method can be used for the rapid quality control of Qingre Zhili Pills.
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Objective:To establish an HPLC method for the determination of palmatine hydrochloride and berberine hydrochloride in Baishi Shuitiao Powder simultaneously. Methods:A reversed phase ion pair HPLC method was adopted. An Agilent Zorbax SB-C18 (150 mm × 4. 6 mm,5 μm)column was used, the mobile phase consisted of acetonitrile-0. 1％ phosphoric acid (50 :50) (0. 2 g do-decyl sodium sulfate added to 100 ml solution), the flow rate was 1. 0 ml·min-1, the detection wavelength was at 345 nm, the injec-tion volume was 10 μl, the column temperature was at room temperature. Results: A good linear correlation was observed within the range of 1. 11-22. 16μg·ml-1 for palmatine hydrochloride (r=0. 9996) and 2. 11-42. 24μg·ml-1 for berberine hydrochloride (r=0. 9998). The average recovery was 98. 94％ with RSD of 2. 43％ for palmatine hydrochloride and 101. 3％ with RSD of 2. 05％ for berberine hydrochloride (n=6). Conclusion:The method is rapid, simple and accurate, and can be used for the content determina-tion of palmatine hydrochloride and berberine hydrochloride in Baishi Shuitiao Powder.
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Objective To observe the antibacterial effects of amikacin sulfate combined with the ingredient of coptis chinensis:the extract of coptis chinensis, berberine hydrochloride and palmatine hydrochloride on multiple drug resistance (MDR) of Escherichia coli (E.coli) in vitro. Methods One hundred strains of E.coli checked out from 2013 to 2014 that showed resistence to cefotaxime were selected, and in which MDR to bacteria were determined. The extended-spectrum β-lactamases (ESBLs)-producing by Kirby-Bauer test. The minimum inhibitory concentrations (MIC) of the extract of coptis chinensis, berberine hydrochloride, palmatine hydrochloride and amikacin sulfate on ESBLs-producing E.coli were determined firstly, and then the sterilization effects of amikacin sulfate combined with the other three medicines were observed by broth microdilution checkerboard method together with their fractional inhibitory concentrations (FIC), with ATCC 25922 for quality control strains. Results Ten MDR E.coli were screened and proved to be ESBLs-producing. The inhibitory effects were enhanced in a synergistic or additive pattern when amikacin sulfate combined with the extract of coptis chinensis, berberine hydrochloride on nine of the ten MDR E.coli in vitro, where the inhibitory effects were a synergistic or additive pattern when amikacin sulfate combined with palmatine hydrochloride on all of the MDR E.coli in vitro. Conclusion Palmatine hydrochloride or berberine hydrochloride or the extract of coptis chinensis combined with the amikacin sulfate has significant value in treatment of MDR E.coli, which is worthy of further study.
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Objective: To establish a quantitative analysis of multi-components by single marker (QAMS) for the simultaneous determination of six alkaloids in crude and processed Coptidis Rhizoma. Methods: An HPLC method was established to determine the six alkaloids (jatrorrhizine hydrochloride, columbamine hydrochloride, epiberberine hydrochloride, coptisine hydrochloride, palmatine hydrochloride, and berberine hydrochloride) by the external standard method (ESM). With this HPLC method, the berberine hydrochloride was used as the internal standard (IS) to determine five relative correction factors (RCFs) of the five other alkaloids, and their contents in all samples were calculated by their RCFs at the same time. Compared with the content results determined by the ESM and QAMS, the feasibility and accuracy of QAMS method were verified. Results: Within a certain range, the RCFs of jatrorrhizine hydrochloride, columbamine hydrochloride, epiberberine hydrochloride, coptisine hydrochloride, and palmatine hydrochloride to berberine hydrochloride were 1.131, 0.999, 1.011, 1.076, and 1.025, respectively, with the good repeatability in different experimental conditions. There was no significant difference between the QAMS method and ESM method. Conclusion: The QAMS method is feasible and accurate for the simultaneous determination of the six alkaloids in crude and processed Coptidis Rhizoma.
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Objective: To establish HPLC method for the simultaneous determination of protopine, palmatine hydrochloride, berberine hydrochloride, dehydrocorydaline, tetrahydropalmatine, tetrahydroberberine, and corydaline in Cuyanhusuo Granule. Methods: The analysis was performed on Ultimate AQ-C18 column (250 mm×4.6 mm, 5 μm) by gradient elution of acetonitrile-0.1% phosphoric acid (adjust to pH 6.0 with triethylamine) (10:90). The UV detection wavelength was set at 280 nm and the flow rate was 1.0 mL/min. Results: The linear ranges of protopine, palmatine hydrochloride, berberine hydrochloride, dehydrocorydaline, tetrahydropalmatine, tetrahydroberberine, and corydaline were 6.8-119.0 (r=0.9999), 24.38-426.65 (r=0.9999), 8.88-155.40 (r=0.9999), 77.66-1359.05 (r=0.9999), 41.4-724.5 (r=0.9999), 6.70-117.25 (r=0.9999), and 25.50-446.25 ng (r=0.9999). The average recoveries (n=6) were 98.2% (RSD=2.0%), 99.6% (RSD=2.8%), 100.2% (RSD=1.3%), 99.0% (RSD=2.2%), 100.8% (RSD=2.6%), 98.7% (RSD=2.5%), and 97.7% (RSD=2.2%), respectively. Conclusion: This method is simple and rapid, and can be used for the quality control of Cuyanhusuo Granule with satisfactory separation and repeatability.
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Objective: To study the content difference of berberine hydrochloride, palmatine hydrochloride, jatrorrhizine hydrochloride, and paeoniflorin in Wujiwan traditional decoction, granule prescription, and compound granule using HPCE internal standard method. Methods: Capillary zone electrophoresis (CZE) method was used for a complete separation of the components, which was achieved with 50 mmol/L borax buffer-methanol (2:1), constant voltage of 25 kV, pressure injection 5 kPa × 15 s, electrolyle sealing 5 kPa × 10 s, and column temperature of 15°C. Results: The capillary electrophoresis method is simple and accurate. The contents of the three alkaloids in the granule prescription were obviously higher than those in traditional decoction and compound granule. Conclusion: This method is instructive for clinical application and quality control of Wujiwan prescription and compound granule.
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AIM: To investigate the changes of alkaloid in Rhizorrm Coptidis and Fructus Evodiae before and after combination. METHODS: The content of berberine hydrochloride,palmatine hydrochloride,jatrorrhizine hydrochloride in Rhizoma Coptidis and Fructus Evodiae before and after combination were determined by TLCS.RESULTS : After combination of Rhizoma Coptidis and Fructus Evodiae,contents of berberine hydrochioride,palmatine hydrochloride,jatrorrhizine hydrochloride significantly reduced,among which the reduction of berberine hydrochloride was more obvious.CONCLUSION: In decoction,Fructus Evodiae appears to restrict the alkaloid from Rhizoma Coptidis in order to lower the side effect of Rhizoma Coptidis.
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Objective To establish a HPLC method for determining of the content of palmatine hydrochloride in Fuke Qianjin Tablets. Methods HPLC was performed on Shimadzu-C18 column. The mobile phase consisted of 0.05 mol·L-1 sodium acid phosphate (pH=3, adjusted by phosphoric acid)-acetonitrile (72 : 28). The detection wavelength was at 265 nm. Results The linear correlation was in the range of 0. 051 μg～0. 255 μg(r=0. 999 9). The average recovery was 100. 04 %, and RSD=1.03 % (n=5). Conclusion The method is accurate and specific.
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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 investigate the transfer rate of alkaloids in extraction and purification process of Cortex Phellodendri Amurensis (CPA) and to ascertain the optimal purification technology.Methods We purified the alkaloids from Cortex Phellodendri Amurensis by AB-8 macroporous resin.With the contents of berberine hydrochloride and palmatine hydrochloride as the reference indexes,content determination of alcohol extract,sample solution and eluent from AB-8 macroporous resin were determined by HPLC.Results The optimal technology was as follows:using 8-fold 75 %(V/V) ethanol as extract,extracting for 3 times and lasting one hour for each time.The transfer rate of alkaloids was 83.75 %under the above condition.The transfer rate of alkaloids was about 80 %when the concentration of sample solution(pH value being 8 and centrifugation) was 0.1 g/mL,and the transfer rate of alkaloids in eluent was 75.14 %.Conclusion The optimum technology is stable and feasible,and the purification effect of alkaloids from Cortex Phellodendri Amurensis by AB-8 macroporus resin is good.
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Objective To establish a method for the content determination of the free anthraquinones,garlic acid,berberine hydrochloride and palmatine hydrochloride in Shuangbai San,and to provide a reference for the quality control and chemical analysis of Shuangbai San.Methods HPLC with Eclipse XDB C18 column was used for the determination of the free anthraquinones.The chromatographic conditions were as follows:methanol-0.1 %phosphoric acid as a mobile phase in gradient mode and detection wavelength at 254 nm,flow rate at 1 mL?min-1,and column temperature at 30 ℃.The chromatographic conditions for the determination of gallic acid were as follows:Nucleodur C18 Gravity column,methanol-0.1 %phosphoric acid solution(2 ∶98) as mobone phase,detection wavelength at 273 nm,flow rate at 1 mL?min-1,and column temperature of 40 ℃.The chromatographic conditions for the determination of berbertine hydrochloride and palmatine hydrochloride were as follows.Nucleodur C18 Gravity,acetonitrile-0.1 %phosphoric acid(every 100 mL solution containing sodium dodecyl sulfonate 0.1 g)(39 ∶61) as mobile phase,detection wavelength at 345 nm,flow rate at 1 mL?min-1,and column temperature being 40 ℃.Results The calibration curves were linear(r≥0.999 7),and the average recoveries were all between 95 %～105 %.The total content of free anthraquinones was 5.1172～5.4933 mg?g-1,the content of gallic acid was 1.3376～2.0673 mg?g-1,and that of berbertine hydrochloride and palmatine hydrochloride were 1.2812～1.6855 mg?g-1.Conclusion This method is reliable and simple,which can provide a reference for the quality control and chemical analysis of Shuangbai San.
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Objective To compare the contents of berberine,palmatine,jatrorrhizine,baicalin and geniposide between traditional decoction and dispensing granule decoction of Huanglian Jiedu Decoction.Methods A HPLC method was carried out on Diamonsil C18 column(250 ? 4.6 mm,5 ?m).The mixture of H2O(A),CH3OH(B)and 0.05 % H3PO4 solution(C)was used as the mobile phase for gradient elution.The column temperature was set up at 35 ℃ and the flow rate was l mL/min.The detection wavelength was 345nm for berberine,palmtine and jatrorrhizine,280 nm for baicalin,and 238 nm for geniposide.Results This method can be used to determine 5 components in Huanglian Jiedu Decoction at the same time and the method was rapid,sensitive and accurate.Conclusion The HPLC chromatograms of traditional sliced decoction of Huanglian Jiedu Decoction are similar to the dispensing granule decoction.The contents of 5 main components in dispensing granule decoction are higher than those in traditional sliced decoction.
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Object To develop a method for the determination of palmatine hydrochloride and berberine hydrochloride in Chinese Mahonia Stem from different habitats Methods HPLC method was set up, using Intersil ODS 3 C 18 column, the mobile phase was acetontrile water sodium laurylsulfonate (470∶ 530∶1 g), the UV detection wavelength was 265 nm, with a flow rate of 1 0 mL/min at 40 ℃ Results A good linearity was obtained in the range of 4 368 52 416 ?g/mL(r=0 999 9) for palmatine hydrochloride and 4 532 54 384 ?g/mL (r=0 999 9) for berberine hydrochloride The average recovery of palmatine hydrochloride and berberine hydrochloride was 98 97% and 98 98%, respectively Conclusion The method is simple, rapid and with better reproducibility for the determination of palmatine hydrochloride and berberine hydrochloride in Chinese Mahonia Stem
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Objective To establish a HPLC method for determining of the content of palmatine hydrochloride in Fuke Qianjin Tablets. Methods HPLC was performed on Shimadzu-C18 column. The mobile phase consisted of 0.05 mol? L-1 sodium acid phosphate (pH=3, adjusted by phosphoric acid)-acetonitrile (72 ∶ 28). The detection wavelength was at 265 nm. Results The linear correlation was in the range of 0.051 ? g～ 0.255 ? g(r=0.999 9). The average recovery was 100.04 % , and RSD=1.03 % (n=5). Conclusion The method is accurate and specific.
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Objective To develop a method for the determination of berberine hydrochloride,palmatine hydrochloride and jatrorrhizine hydrochloride in Yiqi Zhixue Granules. Methods The samples were extracted by ultrasonication with methanol for 30 min,and an ion pair RP-HPLC method was applied to determine three kinds of alkaloids.The column of C18 with temperature at 30 ℃ was used to separate the target components,the mobile phase consisted of the mixed solution of 0.01 mol/L sodium-heptanesulfonate solution and equal volume of 0.01 mol/L potassium dihydrogen phosphate solution(pH being adjusted at 3.1 with phosphoric acid) combined with acetonitrile(70 ∶ 30),the flow rate was 1.0 mL/min,and the detection wavelength was at 345 nm. Results Three kinds of alkaloids were separated perfectly,the average recoveries(n=6)were 100.95 %(RSD=2.10 % ) for berberine chloride,102.14 %(RSD=2.29 % ) for palmatine chloride,and 100.71 %(RSD=2.65 % ) for jatrorrhizine chloride. Conclusion The developed method is demonstrated to be simple,specific and accurate,which can be used to determine the contents of berberine chloride,palmatine chloride and jatrorrhizine chloride in Yiqi Zhixue Granula,and to control the quality of Folium Mahoniae in Yiqi Zhixue Granules.
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Objective To determine the concents of palmatine hydrochloride and berberine hydrochloride in the preparation of Fu Yan Xiao Lotion(FYXL).Methods The HPLC method was established for the determination of palmatine hydrochloride and berberine hydrochloride in the preparation of FYXL.The chromatographic column is Agilent Extend C18(4.6mm? 150 mm,5 ? m),mobile phase consists of water-acetonitrile(40 ∶ 60,3.5 g potassium dihydrogen phosphate and 1.5 g sodium dodecyl sufate per 1 000 mL),column tempreture was 30 ℃,and the flow rate was 1.0 mL/min.The detection wavelength was 345 nm.Results A good linearity is obtained in the range of 0.062 5 ? g to 1.250 ? g of berberine hydrochloride,and 0.068 6～ 1.372 ? g of palmatine hydrochloride.The average recovery of berberine was 98.63 %,RSD being 2.01 %.The average recovery of palmatine was 102.34 %,RSD being 1.67 %.Conclusion This method is simple and quick,and can be used for the quality control of FYXL.
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AIM: To establish the method for determination of gentiopicrin, palmatine hydrochloride and berberine hydrochloride in Ertong Ⅱ Oral Liquid (Cortex Phellodendri, Radix Gentianae, Rhizoma Anemarrhenae, etc.) by RP HPLC. METHODS: The column was a Diamonsil TM C 18 column (250mm?4.6mm, 5?m); the mobile phase was CH 3CN H 3PO 4 C 6H 15 N H 2O; The ultraviolet detection was set at 270nm; the flow rate was 1mL?min -1 . RESULTS: The linear ranges of gentiopicrin, palmatine hydrochloride and berberine hydrochloride were 72.8～728?g?mL -1 ( r=0.9998 ), 7.55～75.5?g?mL -1 ( r=0.9998 ), 12.45～124.5?g?mL -1 ( r = 0.9999 ), respectively. The average recoveries ( n =6) of gentiopicrin, palmatine hydrochloride and berberine hydrochloride were 98.17%, 98.78%, 98.60%; RSD were 1.60%, 1.35%, 1.25%, respectively. CONCLUSION: The method is accurate, reproducible and highly selective, thus suitable for quality control of Er Tong Ⅱ Oral Liqual.