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机构地区:[1]江西中医药大学现代中药制剂教育部重点实验室,江西南昌330004 [2]江西中医药大学中药资源与民族药研究中心,江西南昌330004
出 处:《中国中药杂志》2015年第10期1855-1859,共5页China Journal of Chinese Materia Medica
基 金:中药国家药品标准提高暨2015版药典科研任务;国家自然科学基金项目(30960495)
摘 要:完善凤尾草药材质量标准,提高凤尾草药材及制剂质量控制水平。参照《中国药典》2010年版附录相关方法,对凤尾草药材的水分、总灰分、酸不溶性灰分及醇溶性浸出物进行测定。以硅胶GF254为薄层板,三氯甲烷-甲醇-乙酸(6∶1∶1)为展开剂,以蕨素C-3-O-β-D-葡萄糖苷为对照,紫外光灯254 nm下检视,建立薄层鉴别方法。采用HPLC建立了野漆树苷的含量测定方法。采用Diamonsil C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.15%甲酸水溶液(16∶84)为流动相洗脱,流速1.0 m L·min-1,检测波长350 nm,柱温30℃,进样量10μL。结果表明,在以上薄层色谱条件下,蕨素C-3-O-β-D-葡萄糖苷分离良好。在以上HPLC条件下,野漆树苷在0.025 5~5.1μg线性关系良好,线性回归方程为Y=1 092.4X+9.503 5(r=0.999 8),平均加样回收率为100.3%(RSD 1.3%)。16批凤尾草药材的测定结果表明,野漆树苷的质量分数为0.08~5.06 mg·g-1,水分为7.35%~12.96%,总灰分为6.90%~16.33%,酸不溶灰分为2.07%~11.38%,醇溶性浸出物为13.29~23.87%。建议规定凤尾草的水分不得超过12%,总灰分不得超过15%,酸不溶灰分不得超过8.5%,醇溶性浸出物不得少于14%,以干燥品计算,野漆树苷含量不得少于0.040%。结果表明建立的凤尾草质量标准具有很好的专属性和准确性,可用于凤尾草药材的质量控制。The quality control method and standard were established to control the quality of Pteris multifida in this paper. The tests of water content, total ash, acid-unsoluble ash and ethanol-soluble extractives of P. multifida were carried out according to the methods recorded in appendix of Chinese Pharmacopeia(2010 edition,volume 1 ) . The TLC method was established by using rhoifolin as references ,and a mixture of CHC13-MeOH-HAc( 6: 1:1 ) as the developing solvent system on GF254 thin layer plate. The contents of rhoifolin was determined by HPLC on a Diamonsil C18 (4. 6 mm × 250 mm, 5 μm) column, using acetonitrile-water( containing 0. 15 % formic acid) ( 16: 84) as mobile phase at a flow rate of 1. 0 mL ~ min-1. The column temperature was 30 ℃ and the detection wavelength was 350 nm. As a result,pterosin C 3-O-β-D-glucosidede and the other constituents were well separated on TLC detected under the UV light at 254 nm. The methodology validation for the assay of rhoifolin presented that it was in good linear correlation in the ranges of 0. 025 5-5.1 μg with the regression equations of Y = 1 092.4X + 9. 503 5 ( r = 0. 999 8 ), and the average recoveries were 100. 3% ( RSD 1.3% ). The content range of rhoifolin from 16 different batches of Pteris multifida was 0. 08-5.06 mg · g^-1. The water content, total ash, acid-unsoluble ash and ethanol-soluble extractives of 16 samples varied in the ranges of 7.35%-12. 96%, 6. 90% -16. 33%, 2. 07%-11.38% and 13.29%-23.87% ,respectively. The suggesting limes in the quality standard for water content,total ash, acid-unsoluble ash, ethanol-soluble extractives and rhoifolin content were ≤12%, ≤15% , ≤8.5%, ≥14% and ≥0. 040%, respectively. The result proved that the established quality of control method was specific and accurate ,which can be used for the quality control of P. multifida.
关 键 词:凤尾草 质量标准 蕨素C-3-O-β-D-葡萄糖苷 野漆树苷
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