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OBJECTIVE： To establish a method for content determination of N-（E）-p-coumaroyltyrosine in leaves of Abrus cantoniensis， and to optimize its purification technology. METHODS： HPLC method was adopted for the content determination of N-（E）-p-coumaroyltyrosine in A. cantoniensis. The determination was performed on Hypersil BDS C18 column with mobile phase consisted of 0.1％ formic acid water （A）-methanol （B） （gradient elution） at a flow rate of 1.0 mL/min. The column temperature was set at 25 ℃. The detection wavelength was set at 300 nm， and sample size was 10 μL. Using polyamide resin as material， the yield of N-（E）-p-coumaroyltyrosine as indicators， single factor test was used to optimize the purification technology of N-（E）-p-coumaroyltyrosine， such as concentration， sample size， stationary adsorption time. RESULTS： The linear range was 2.575-51.50 μg （r＝0.999 9） for N-（E）-p-coumaroyl-tyrosine. The limit of quantification was 0.000 618 μg， and the detection limit was 0.000 129 μg. RSDs of precision， stability and reproducibility tests were all lower than 3％. The recoveries were 97.04％-102.43％ （RSD＝2.06％， n＝6）. The optimal purification technology was as follows： the concentration of the sample solution was 0.04 g /mL （by the leaves of A. cantoniensis）； sample capacity 50 mL； the sample flow rate was 1.0 mL/min； the stationary adsorption time was 20 min； the eluting solvents were ammonia containing water （containing 0.1％ acetic acid）， 20％ ethanol （containing 0.1％ acetic acid） and ammonia（pH 10）. Average yield was 98.94％，average dry paste content was 61.17 mg/g， and average dry paste purity was 19.73％ by optimal purification technology. CONCLUSIONS： Established method is simple， accurate and stable. The optimized technology is stable and feasible.
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[Objective] To compare the difference of fingerprints of Pogostemon cablin (Blanco) Benth. from different places of origin. [Methods] The chemical components of Pogostemon cablin (Blanco) Benth. from 6 places of origin were detected by thin-layer chromatography. [ Results ] The thin-layer chromatogram of volatile components of Pogostemon cablin (Blanco) Benth. from different places of origin was similar. The contents of methanol-extract and petroleum-ether-extract from Pogostemon cablin (Blanco) Benth. planted in Gaoyao, Guangdong differed greatly from those in other places of origin, which can be used to identify the herb of Pogostemon cablin ( Blanco) Benth. from Gaoyao, Guangdong. [Conclusion] Thin-layer chromatographic fingerprints can be used as the parameter to differentiate Pogostemon cablin (Blanco) Benth. from different places of origin.
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【Objective】 To assay the naringenin content in different medicinal materials of Exocarpium Citri Grandis (ECG). 【Methods】 High performance liquid chromatography (HPLC) was applied to determine the naringenin content in different medicinal materials of ECG. The chromatographic conditions were: gradient elution being performed with methanol as mobile phase A and water - acetic acid (61: 4) as mobile phase B, flowing rate being 1.0 mL/min; detecting wavelength at 283 nm. 【Results】 In the rage of 0.088～0.880 ?g, naringenin showed a good linearity with the chromatographic peak area, r=0.9999, average recovery rate was 95.49% and RSD=2.00% (n=5). The naringenin content in 23 different samples of ECG was in the range of 0.1～1.0 mg?g~(-1). 【Conclusion】 It is the first time to establish the HPLC method for the determination of naringenin content in ECG and the method is accurate and reproducible. Naringenin content in varieties of ECG is stable and the difference of naringenin content between Citrus grandis Osbeck. Var. tomentosa Hort. and Citrus grandis (L.) Osbeck is not significant.
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[Objective] To assess the quality of Citrus grandis Osbeck. Var. tomentosa Hort. (CGO Var. TH) and Citrus grandis (L. ) Osbeck (CGO). [Methods] The macroscopic feature and microscopic structure of CGO Var. TH and CGO were compared. Their content of total flavones (TF) was determined by spectrometry, naringin content and fingerprint by high performance liquid chromatography (HPLC) and the content of rhoifolin by thin-layer chromatography (TLC). Their expectorart, anti-inflammatory and antitussive effects were observed by phenol red test, auricular swelling test and ammonia-water-induced cough method. [Results] Obvious differences such as villi in the exocarp and non-grandular hair in the stem existed in the macroscopic feature and microscopic structure of CGO Var. TH and CGO. The contents o{ total flavones and naringin in CGO Var. TH were markedly higher than that in CGO and the rhoifolin content in CGO Var. TH was ten times as much as that in CGO. Markedly difference was also found in their fingerprint. The expectorant, anti-inflammatory and antitussive effects in CGO Var. TH were better than those in CGO. [Conclusion] The quality of CGO Var. TH is much better than that of CGO.
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Objective To establish a method for the determination of Rhoifolin content in Exocarpium citri grandis (ECG). Methods The RP-HPLC method was operated on MACHEREY-NAGEL 100-5 C_(18), with methanol and wateracetic acid (61: 4) as mobile phase, gradient elution, flow rate at 1.0 mL/min, and detection wavelength at 345nm. Results In the range from 0.816 ?g to 13. 056?g, Rhoifolin is in a good linearity with chromatographic peaks area, r=0.9995, the average recovery ratio is 101.064%, RSD=3.10%(n=5). The content of Rhoifolin in Tomentulosus Exocarpium Citri Grandis(TECG) ranged from 1.33% to 0.177% and that in Glabrous Exocarpium Citri Grandis (GECG) is less than 0.17%. Conclusions RP-HPLC method is with accuracy and a good reproducibility for the determination of the Rhoifolin content in ECG; the difference of Rhoifolin content in TECG and GECG is significant.
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Objective: To establish a method for determinating icarin content in Naoling Granule. Methods: Water-soluble ethyl-acetate-extracting polyamide column purification was adopted. The content of icarin was determined by HPLC. C18 column was used, mobile phase was methanol:0.1mol/mL sodium phosphate dibasic (6:5) and detection wavelength was at 270nm. Results: Icarin has a good linearity in the range of 0.24～1.2?g ( r=0.9998). The average recovery was 98.23 %and RSD was 1.2 %(N=5). Conclusion: The method was simple with good reproducibility and can be used for the content determination of icarin in Naoling Granule.
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Objective To study the influence of different dosage forms on the release rate of total salvianolic acid of sus- tained-released Danshen extract preparations.Methods With salvianolic acid B as the standard,uhraviolet spec- trophotometry and the release test were applied to determine the accumulated release rate of total salvianolic acid of sus- tained-released Danshen extract preparations(R1～R9)of 9 different dosage forms and to evaluate the release behav- ior of sustained-released Danshen extract preparations in vitro.Results The accumulated release rate of total sal- vianolic acid in R7 was the best,and the in vitro release behavior was consistent with Higuchi equation:M_1/M_∞= 0.363 4t~(1/2)-0.1656,r= 0.996 2.Conclusion R7 is the first choice dosage form for the preparation of the sus- tained-released Danshen extraction preparations.
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Objective To establish the method for determination of astragaloside Ⅳ in Fufang Buqi Yangxue Oral Solution by RP-HPLC.Methods The content of astragaloside Ⅳ was determined by a HPLC system under the following conditions:the chromatographic column was Agilent C18(150 mm? 4.60 mm,5? m),the mobile phase was acetonitrile-water(60:40),the flow rate was 1.0 mL? min-1,and the detection wavelength was at 203 nm.Results Astragaloside Ⅳ showed good linearity in the range of 0.34～ 3.40 ?g(r=0.999 9).The average recovery was 100.8 %,and RSD was 1.47 %(n=6).Conclusion The HPLC method is simple and reproducible,and can be used for quality control of Fufang Buqi Yangxue Oral Solution.
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Objective To establish a method for the determination of berberine hydrochloride in Siji Sanhuang capsules(SSC).Methods The RP-HPLC method was performed on Agilent Hypersil ODS column(4.6 mm?150 mm,5 ?m).Acetonitrile and 0.05 mol/L NaH2PO4 water(adjust pH to 3 with H3PO4)were used as the mobile phase(30 ∶70),detection wavelength was at 270 nm,the flow rate was 1.0 mL/min and the column temperature was at 25 ℃.Results In the range of 0.094 to 0.470 ?g,berberine hydrochloride had a good linearity with chromatograph peaks area(r=0.998 3),the average recovery ratio was 98.5 %(n=5),and RSD=2.3 %.Conclusion This method is simple,effective and with a higher sensibility and stability.The method can be used to control the quality of SSC effectively.
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Objective To study the fingerprint determination method of Pogostemon cablin by HPLC.Methods A RP-HPLC method was established with the mixed solution of methnol and 0.1 % acetic acid aqueous solution as mobile phase(gradient elution),flow rate at 1.0 mL/min,detection wavelength at 254 nm,analytic time being 50 min and column temperature at 25 ℃.Results The results of comparative analysis of 10 batches samples showed that 15 common peaks were shared by Pogostemon cablin.The common peaks were classified to two regions and the second was the main characteristic region which had an amount of characteristic peaks.All samples had the similar fingerprint features.Conclusion The method is accurate,repetitive and can be applied for the identification and quality control of Pogostemon cablin.
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Object To establish a new method to determine protocatechualdehyde in Maodongqing Sustained- release Tablet. Methods The RP- HPLC method was applied with CH3OH and 1 % acetic acid as mobile phase, flowrate at 1.0 mL/min, and detection wavelength at 312 nm. Results In the range from 11.7 ng to 140.4 ng, protocatechualdehyde was in a good line with peak area, r=0.99995, the average recovery ratio was 96.41 % , RSD=1.04 % (n=5). Conclusions It was the first time to establish the RP- HPLC method to determine and control the protocatechualdehyde in Maodongqing Sustained- release Tablet with accuracy and a good reproducibility.
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Objective To determine the appropriate collecting -time of Exocarpium citri grandis,the chemical compo-sition in Exocarpium citri grandis in different fruit -ages was compare d and analyzed.Methods Contents of naringein and bergapten were compared by TLC an d the total dihydroflavones in Exocarpium citri grandis was determined by spec-trophotometmic analysis with detection wavelength at 384nm.Results With the increase of fruit -age,the c ontents of naringein and total dihydroflavones in Exocarpium citri grandis decreased and the content of bergapt en increased.Con-clusion Fruit -age has an obviously effect on the chemical composition in Exocarpium citri grandis and collecting -time can influence the quality of medicin e materials.Further studies of Exocarpium citri grandis should be combined pharma-codynamics for fixing collecting -t ime.