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Objective To optimize the manufacture process for Zhibai Anshen oral liquid. Methods The orthogonal designed experiments were conducted to monitor the effects of three factors on the content of mangiferin. The three factors included the amount of water, extraction time and alcohol precipitation concentration. Six month accelerated stability study and twelve month long term stability study were performed. Results Optimum percolation process was boiling the mixture with 10 times of water for 1 hour, followed by deposition with 60% alcohol. Conclusion This optimized process can be used for mass production.
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Objective To establish a quality control standard for Qingre Baidu granules .Methods Isatidis Radix ,Fruc-tus Forsythiae ,Herba Violae ,and Glycyrrhizae were identified by TLC ,and the concentration of chlorogenic acid was deter-minedbyHPLC.ThismethodwasemployedonanAgilentZORBAXSB-C18column(4.6mm×250mm,5μm)at30℃ witha mobile phase of acetonitrile (A) and 0 .2% formic acid (B) using the gradient elution program shown as follows :0-12 min , 11%-12% A run at the flow rate of 1 .0 ml/min .The injection volume was 20 μl and the detection wavelength was 327 nm . Results Characteristic spots could be detected by TLC and the specificity of the method was satisfactory .As for chlorogenic acid ,the equation of linear regression of chlorogenic acid was Y=60 .239 4X+9 .096 3 (r=0 .999 9) with the linear range of 6.19-396 .00 μg/ml .The average recovery was 99 .66% (RSD=2 .82% ) .Conclusion The established method is simple ,reli-able ,reproducible ,and can be used for the quantitative determination and quality control of Qingre Baidu granules .
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Objective To establish a high performance liquid chromatography method for the determination of matrine in Lefu oral liquid .Methods The HPLC method was performed on a Diamonsil Platisil NH2 column (4 .6 mm × 250 mm ,5μm) with the mobile phase of acetonitrile-isopropyl alcohol-3% phosphoric acid solution (84 ∶ 4 ∶ 12 ) . The flow rate was 1 .2 ml/min .The sample injection volume was 5 μl .The detective wavelength was 205 nm .Results The calibration curve of matrine showed good linear response ranged from 54 .50 to 872 .00 μg/ml with r=0 .999 1 .The average recovery of spiked samples for matrine was 99 .82% while the relative standard deviation for repetitions was 1 .12% .Conclusion The method was simple ,reliable and repeatable ,which could be used for the quantitative determination of matrine of Lefu oral liquid .
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Objective To establish quality control of Xinnaoling granules .Methods Thin layer chromatography (TLC) methods were used to identify Rhizoma Corydalis ,Radix Angelicae dahuricae ,Cortex Magnoliae officinalis ,Radix Glycyrrhi-zae ,Rhizoma Ligusticum ,Ligusticum wallichii ,Schisandra Chinensis ,Dendranthema morifolium .The concentration of salvi-anolic acid B was determined by high performance liquid chromatography (HPLC) .The method employed a column of Agilent Eclipse XDB-C18 (4 .6 mm × 250 mm ,5 μm) with a mobile phase of 0 .5% formic acid (A)-acetonitrile (B) at a temperature 25℃ .The gradient elution program was as follow :0~5 min 24% B ,5~6 min 24% ~19% B ,6~25 min 19~20% B .The flow rate was 1 .0 ml/min ,and the injection volume was 10μl and the detection wavelength was 286 nm .Results The spots in TLC plates were clear and specific .As for salvianolic acid B ,the linear range was 20-1 280 μg/ml and the equation of linear regres-sion of salvianolic acid B was Y=13 .304 X -117 .50 (r=0 .999 9 ,n=7) .The average recovery rate was 96 .17% (RSD=1 . 10% ) .Conclusion The method was proved to be simple ,reliable ,reproducible ,and could be used in the quality control of Xinnaoling g ranules .
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Objective To study the fingerprint of Polygonum cuspidatum from various regions by HPLC and provide technical support for the identification.Methods HPLC conditions :the chromatographic column was Agilent ZORBAX SB-C18 (4.6 mm × 250 mm,5 μm);the mobile phase was 0.1% formic acid in water and acetonitrile (A-B);gradient elution ;the de-tection wavelength was 306 nm ;the flow rate was 1 ml/min;the column temperature was 30 ℃ ;injection volume was 20 μl. Results The HPLC gradient conditions could effectively separate polydatin,resveratrol,emodin and emodin ether,etc.Con-clusion This method is stable,effective and durable,which is instructive to the herbs data identification of Polygonum cuspi-datum.
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Objective To establish the quality standard for Quban oral liquid .Method Thin layer chromatography (TLC)was used for quality identification of Codonopsis pilosula ,Astragalus membranaceus ,Paeonia veitchii ,Paeonia lacti‐flora,AtractylodesmacrocephalaandAngelicasinensis.ThepaeoniflorinwasdeterminedbyRP‐HPLC.Result Clearspots were obtained with good separation in TLC identification which was highly specific .The paeoniflorin area and content showed a good linear relationship at the range of 18 .20‐2 330 .00 μg/ml (r= 0 .999 9) .The average recovery was 99.72% (RSD=1.25% ) .Conclusion This method is simple ,rapid ,accurate ,and which can be used for the quality control of Quban oral liquid .
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Objective To establish quality standards forAnshu Liquid.Methods Phellodendri Chinensis Cortex and Kochiae Fructus were qualitatively identified by TLC method. The contents of berberine hydrochloride and phellodendrine hydrochloride in the preparation were determined by HPLC method. The chromatographic column was ZORBAX SB-C18 (4.6 mm×250 mm, 5μm); the mobile phase was acetonitrile-0.1% phosphoric acid (0.5% diethylamine) gradient elution; the flow rate was 1.0 mL/min; the detection wavelength was 284 nm.Results Berberine hydrochloride and phellodendrine hydrochloride in Phellodendri Chinensis Cortex and saponin Ic in Kochiae Fructus were detected by TLC method. The linear relationship of berberine hydrochloride in the preparation was Y=23.109X?30.548,r2=0.999 8, RSD=2.97%, showing that the linear range of berberine hydrochloride was 0.050 5– 2.525 0 μg. The linear relationship of phellodendrine hydrochloride in the preparation wasY=10.038X?2.446 6, r2=0.999 9, RSD=1.24%, showing that the linear range of phellodendrine hydrochloride was 0.050 0–2.500 0 μg. Conclusion The method is accurate, rapid, stable and reliable, with good reproducibility, which can be used for the quality control and evaluation ofAnshu Liquid.
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Objective To establish a quality standard forZishen Tongguan Capsules.Methods Anemarrhneae Rhizoma and Phellodendri Chinensis Cortex were qualitatively identified by TLC method. The contents of neomangferin, phellodendrine hydrochloride, mangiferin and berberine hydrochloride inZishen Tongguan Capsules were quantitatively determined by HPLC method.Results The spots of qualitative identification method were clear without interference. Neomangferin in Anemarrhneae Rhizoma and phellodendrinehy drochloride in Phellodendri Chinensis Cortex were identified. Neomangferin, phellodendrinehy drochloride, mangiferin and berberine hydrochloride showed good linearity in the range of 0.025 25–2.02 μg (r=0.999 7), 0.025 5–2.04 μg (r=0.999 7), 0.026–2.08 μg (r=0.999 7), and 0.025 5–2.04 μg (r=0.999 6) respectively. The average recoveries of neomangferin, phellodendrinehy drochloride, mangiferin and berberine hydrochloride were 99.99%, 101.06%, 103.05%, and 100.55%, respectively. The RSD were 2.69%, 5.62%, 2.49%, and 2.06%, respectively.Conclusion The method is accurate and rapid, with good stability, reliability and reproducibility, which can be used for the quality control and evaluation of the preparation of Zishen Tongguan Capsules.
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OBJECTIVE:To establish a method for simultaneous determination of 4 psoralen compounds in Buwu tincture. METHODS:HPLC was performed on the column of Dikma Diamonsil C18 with mobile phase of acetonitrile-0.2% Acetic acid by gradient elution at flow rate of 1 ml/min,detection wavelength was 246 nm,column temperature was 30 ℃,and the injection vol-ume was 15 μl. RESULTS:The linear range was 13.00-208 μg/ml for angelicin,26.00-416 μg/ml for bavachin,24.50-392 μg/ml for psoralidin and 37.88-606 μg/ml for isobavachalcone,respectively(r≥0.999 6);RSDs of precision,stability and reproducibility tests were less than 2.00%;recoveries were 95.22%-97.23%(RSD=0.87%,n=6),100.24%-104.64%(RSD=1.62%,n=6), 102.28%-104.39%(RSD=1.47%,n=6)and 97.68%-100.17%(RSD=0.97%,n=6),respectively. CONCLUSIONS:The method is simple and reproducible,and can be used for the quality control of Buwu tincture.
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Objective To establish the quality standards for compound Shatagan Oral Liquid. Methods Chuanxiong Rhizoma was identified by TLC. The content of ferulic acid was determined by HPLC. Separation was performed on a Diamonsil C18 column (4.6 mm × 250 mm, 5μm) with a mobile phase consisting of methanol-1% acetic acid solution in gradient elution (0-5 min, 35% methanol;5-8 min, 35%→23% methanol;8-22 min, 23% methanol) at 30℃;The flow rate was 1.0 mL/min;The injection volume was 5μL;The detection wavelength was 322 nm.Results Ferulic acid showed a good linear relationship in the range of 0.039 4-0.630 0μg (r=0.999 7,n=7). The average recovery was 98.22% and RSD was 2.62% (n=6).Conclusion The method is reliable, sensitive and with repeatability, which can be used as the quality control method for compound Shatagan Oral Liquid.
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OBJECTIVE:To establish the quality standard for Xianrengu oral liquid. METHODS:Thin layer chromatography (TLC) was used for qualitative identification of Epimedii Folium,Astragali Radix,lycium barbarum,Atractylodes macrocephala and Panax ginseng in Xianrengu oral liquid;RP-HPLC was preformed on the column of Dikma Diamonsil C18 with the mobile phase of acetonitrile-0.1% phosphoric acid (30∶70,V/V)at the flow rate of 1.0 ml/min,the detection wavelength was 270 nm,the temperature was 30℃and the volume was 10μl. RESULTS:TLC identification had good separation,clear spots and high specifica-tion. The linear range of icariin was 7.97-510.00 μg/ml(r=0.999 3);RSDs of precision,stability and reproducibility tests were no more than 0.83%;and the average recovery was 97.69%(RSD=1.30%,n=6). CONCLUSIONS:This method is simple,accu-rate and simple,which can be used for the quality control of Xianrengu oral liquid.
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Five compounds were isolated from marine sponge Aplysinopsis sp.collected from the South China Sea.Their structures were elucidated by ~1H-NMR,~(13)C-NMR and MS as (E)-3'-deimino-3'-oxoaplysinopsin(Ⅰ),(Z)-3'-deimino-3'-oxoaplysinopsin(Ⅱ),3-(2- oxopropyl )- 3-hydroxyind-olin-2-one(Ⅲ),1H-indole-3-carboxaldehyde(Ⅳ),5?,6?-epoxystigmasta -7-en-3?-ol(Ⅴ).CompoundsⅢ,Ⅴwere isolated from Aplysinopsis sp.for the first time.