参术补钙颗粒的质量标准研究

The Quality Standard of Shenzhu Calcium Supplem Granule

建立了参术补钙颗粒的质量标准。采用薄层鉴别方法鉴别甘草、党参、白术;采用原子吸收分光光法测定参术补钙颗粒中钙的含量;HPLC法测定参术补钙颗粒中维生素D3的含量。结果表明以三氯甲烷∶乙酸乙酯∶甲醇∶水(15∶40∶22∶10)10℃以下放置的下层溶液作为展开剂,喷10%硫酸乙醇,加热5至10 min,置紫外365 nm下检视可鉴别出甘草;以甲苯∶乙酸乙酯∶甲酸(20∶8∶0.5)为展开剂中展开,喷10%硫酸乙醇,105℃加热可鉴别出党参;以三氯甲烷∶丙酮(19∶1)作为展开剂,置紫外365 nm下检视可鉴别出白术;钙在0~18μg/mL范围内线性关系良好,RSD为1.75%,参术补钙颗粒中所含钙的含量定为8.76 mg/g;维生素D3.在125~100μg/mL范围内线性关系良好,平均回收率为94.83%,RSD为2.77%,参术补钙颗粒中所含维生素D3的含量定为0.0248μg/g。该方法定性定量方法简便、准确、灵敏度高、重复性好,可用于参术补钙颗粒的质量控制。

To develop a quality standard for Shenzhu Calcium Supplem Granule. The licorice, Atractylodes, Codonopsis were identified by thin layer identification;Determination of Vitamin D3 in Shenzhu Bugai Granules by HPLC.Determination of Calcium in Shenshu Bugai Granules by Atomic Absorption Spectrophotometry. The lower layer solution of chloroform∶ethyl acetate∶methanol∶water(15∶40∶22∶10) and 10 ℃ or less was used as a developing solvent, sprayed with 10% sulfuric acid ethanol, heated for 5 to 10 minutes, and examined at 365 nm. Can be identified as licorice;toluene∶ethyl acetate∶formic acid(20∶8∶0.5) as a developing agent, spray 10% sulfuric acid ethanol, 105 ℃ heating can identify Codonopsis;chloroform∶acetone(19∶1) As a developing agent, a white surgery can be identified by viewing at 365 nm. The spots of TLC were clear, which could identify licorice, Codonopsis pilosula and Atractylodes macrocephala in Shenzhu Bugai Granules. The linear relationship of vitamin D3 was good in the range of 3.125~100 μg/mL,and the average recovery rate was 94.83% with RSD of 2.77%. The content of calcium in shenzhu calcium supplement granules was 8.76 mg/g.Calcium has a good linear relationship in the range of 0~18 μg/mL and RSD of 1.75%. The content of vitamin D3 in shenzhu calcium supplement granules was 0.0248 μg/g. The method is simple, accurate and reproducible, and can be used for the quality control of Shenshu Bugai Granules.