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OBJECTIVE：To compare the quality between Stamen typhae and pollen of T. angustifolia ，and provide scientific evidence for the improvement of quality standard of T. angustifolia . METHODS ：Fifteen batches of S. typhae were collected. Pollen minus sieve ，impurity plus sieve （filament and anther ）were sift out from S. typhae according to the identification method of T. angustifolia in Chinese Pharmacopoeia （2015 edition）. The characteristics and components of S. typhae and pollen ，filament and anther of T. angustifolia were comfirmed by impurity ， character examination and microscope ， TLC. The contents of isorhamnetin-3-O-neohesperidoside and typhaneoside in S. typhae and pollen ，impurities plus sieve （filament and anther ）of T. angustifolia were determined by HPLC. RESULTS ：S. typhae was a mixture of pollen ，anther and filament of T. angustifolia ，in the form of brownish yellow flocculent. The pollen of S. typhae was yellow powder with delicate hand feel ，slight smell and light taste；the surface of cells was slightly striped. The filaments and anthers were filiform and short-term ，rough and astringent ，and the cell surface were long strip. TLC chromatogram of S. typhae ，pollen and impurity of T. angustifolia had the same color spots at the same location. The contents of isorhamnetin- 3-O-neohesperidoside，typhaneoside and their aggregate were the highest in pollen （0.42％，0.24％，0.64％）；the second in S. typhae （0.22％，0.17％，0.39％）；the lowest in the impurities plus sieve （0.19％， 0.14％，0.33％）. The total contents of isorhamnetin- 3-O-neohesperidoside and typhaneoside in S. typhae and in impurities plus sieve did not reach the content limit stipulated in Chinese Pharmacopoeia （not less than 0.50％）. CONCLUSIONS：The medicinal components of T. angustifolia mainly exist in pollen. It is suggested that S. typhae should be used as the raw material to obtain pollen，and should not be used directly.
ABSTRACT
Objective: To establish an HPLC method for the simultaneous determination of 3 active components in compound he-mostatic capsules and investigate the content changes before and after 60Co-γ ray irradiation. Methods: An Agilent-C18column (250 mm×4. 6 mm, 5 μm) was adopted and the flow rate was 1. 0 ml·min-1. The mobile phase consisted of acetonitrile-0. 5% phosphor-ic acid solution (triethylamine was used to adjust pH to 6) with gradient elution, the detection wavelength was 254 nm (0-35 min) and 281 nm (35-55 min), and the column temperature was 35℃. The compound hemostatic capsules were irradiated at 5, 8 and 10 kGy, respectively, and the contents of the 3 active components in compound hemostatic capsules were compared before and after the radia-tion,and the t-test was applied to investigate the significance. Results: Typhaneoside,isorhamnetin-3-O-neohesperidin and tetrahydro-palmatine respectively within the concentration range of 0. 018-0. 11 mg·ml-1,0. 020-0. 120 mg·ml-1and 0. 011-0. 066 mg·ml-1 showed a good linear relationship with the peak area. The average recovery was 97. 7% , 98. 7% and 99. 3% with the RSD of 0. 9% , 0. 9% and 0. 5% , respectively (n=6). After the irradiation, the contents of the three active components in compound hemostatic capsules all showed changes. Under the dose of 8 kGy, the content changes of typhaneoside and isorhamnetin-3-O- neohesperidin showed no statistical significance (P>0. 05),and when the dose increased to 10 kGy,the content of tetrahydropalmatine exhibited sig-nificant difference (P<0. 05). Conclusion: The established determination method for compound hemostatic capsule shows such ad-vantages as high recovery, good repeatability, simple operation and promising separation, which can be used as a quality control meth-od for compound hemostatic capsules. The sterilization effect of 60Co-γ ray irradiation on compound hemostatic capsules is significant without notable changes in the active components. When the irradiation dose is equal to or below 5 kGy,the change of each component is not obvious,which can provide reference for the radiation sterilization of compound hemostatic capsules.
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Objective To establish the identification method of Typha angustifolia (stir-bake to black), Sophora japonica, Sanguisorba officinalis (stir-bake to black), and Rheum palmatum in Fuhuang tablets. Methods HPLC method were studied to identify typhaneoside and isorhamnetin-3-O-neoheptanoside in T. angustifolia, and sophoricoside in S. japonica. HPLC conditions were as follows: Agilent TC-C18 (2) column (250 mm × 4.6 mm, 5 μm) with a gradient elution at a temperature of 30 ℃; Phosphate buffer and acetonitrile were used as the mobile phase with a flow rate of 1.0 mL/min; The detection wavelength was 254 nm. The acid hydrolysis-HPLC method was explored to identify S. officinalis (stir-bake to black). TLC identification method was performed to identify R. palmatum. Results HPLC method can identify typhaneoside, isorhamnetin-3-O-neoheptanoside, and sophoricoside synchronously. Acid hydrolysis method can identify S. officinalis (stir-bake to black) by HPLC and TLC can identify R. palmatum. Conclusion The three methods are simple and accurate with high sensitivity and good specificity, which can be used to identify all herbal medicines in Fuhuang tablets.
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Objective To optimize the matrix formulation for Shaofu Zhuyu Cataplasm (SZC) by Plackett-Burman design combined with Box-Behnken response surface method and study its transdermal permeation properties in vitro. Methods In this paper, the appearance description, initial bonding strength, endurance bonding strength, and peel strength were taken as indexes. Based on the result of a single factor experiment, the formula for the SZC was optimized by Plackett-Burman combined with Box-Behnken method. Franz diffusing cells method was chosen to investigate the tansdermal infiltration capacity of SZC with different dosage penetration enhancers of azone in vitro, taking ferulic acid, paeoniflorin, isorhamnetin-3-O-neohesperidin, and typhaneoside as index components. Results NP-700, tartaric acid and kaolin had significant effects on the properties of SZC. The optimal ratio of the prescription was as follows: NP-700-tartaric acid-kaolin (2.42:0.16:0.96). The promoting effect of 3% concentration for index component was better, and the transdermal rates of ferulic acid, paeoniflorin, isorhamnetin-3-O-neohesperidin, and typhaneoside were 6.889 4, 1.917 4, 0.852 0, and 0.893 7 μg/(cm2∙h), respectively. Conclusion The SZC was uniform, without residual behavior in application. And it had a good release and transdermal properties, and transdermal actions were consistent with zero-order kinetics.
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Objective: To study the extraction process of the total flavones of Pollen Typhae ( Typha angustifolia L.). Methods: The optimum extraction process was selected with the orthogonal design. The content of total flavones was determined by UV spectrophotometry. Results: The significant effects of alcohol concentration, extraction time and extraction times on the extraction of total flavones were discovered. Conclusion: The optimum extraction process was as follows: Pollen Typhae was extracted with 70% alcohol for 3 times, with the solvent volume 8, 6, 6 times amount and extraction time 60, 60, 30 minutes in turn.
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Objective: To study the quality standard for Puhuang Dispensing Granule (Pollen Typhae). Methods : Puhuang Dispensing Granule was identified by TLC and isorhamnetin-3-O-neohesperidoside and typhaneoside in Puhuang Dispensing Granule were determined by HPLC. Results : The linear relationship was at the range of 0.4～1.21?g for isorhamnetin-3-O-neohesperidoside and 0.42～1.25?g for typhaneoside, respectively. The average recovery was 98.88% for isorhamnetin-3-O-neohesperidoside and 99.68% for typhaneoside, respectively. Conclusion : The method is available with a good reproducibility and can control the quailty of Puhuang Dispensing Granule.