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机构地区:[1]浙江省舟山医院药剂科,浙江舟山316021 [2]浙江省舟山市食品药品检验所,浙江舟山316021
出 处:《中国药学杂志》2013年第23期2039-2044,共6页Chinese Pharmaceutical Journal
摘 要:目的采用一测多评方法,建立大败毒胶囊中总蒽醌的含量测定方法。方法采用C_(18)柱(4.6mm×250mm,5μm),以甲醇-0.1%磷酸溶液(85:15)为流动相,流速1.0 mL·min^(-1),柱温25℃,检测波长254 nm,建立大黄酸、大黄酚和大黄素甲醚与内标物大黄素间的相对校正因子,并以相对保留时间作为目标峰的定位标准。结果色谱峰分离度良好,大黄酸在5.724×10^(-2)~0.572 4μg、大黄素在4.58 4×10^(-2)-0.458 4μg、大黄酚在6.368×10^(-2)~0.636 8μg、大黄素甲醚在6.548×10^(-2)-0.654 8μg内呈良好线性关系,r(0.999 7~0.999 9),加样回收率大黄酸为(97.8±1.4)%,大黄素为(100.7±1.0)%,大黄酚为(98.6±0.6)%,大黄素甲醚为(97.0±1.4)%。大黄素对大黄酸、大黄酚和大黄素甲醚的相对校正因子分别为1.19,1.40,1.06。结论该方法简单、快速。准确、可靠,可用于大败毒胶囊中蒽醌类成分的质量控制。OBJECTIVE To establish a auantitative analysis of multi-components by single marker(QAMS) method for determi- ning the content of anthraquinones in Dabaidu capsules( traditional Chinese medicines). METHODS The relative correction factors (RCFs) of emodin to rheiM, chrysophanol, and physcion were determined on a Cls column (4. 6 mm x 250 mm, 5~m) with methanol- 0. 1% phosphoric acid (85: 15) as mobile phase. The flow rate was 1.0 mL ~ min-t. The column temperature was set at 25 ~C. The detection wavelength was set at 254 nm. The relative retention time (RRT) was used to define the target peak. RESULTS The cali- bration curves for rheiM, emodin, chrysophanol, and physcion showed good linearity in the ranges of 5. 724 ± 10-2 - 0. 572 4 μg, 4. 584 × 10 -2 _ 0. 458 4μg, 6. 368× 10 -2 _ 0. 636 8μg and 6. 548 × 10 2 -0. 654 8 μg, r(0. 999 7 -0. 999 9), respectively. The recov- eries were (97.8~1.4)%, (100.7±1.0)%, (98.6±0.6)% and (97.0±1.4)%, respectively. The RCFs were 1.19, 1.40 and 1.06. CONCLUSION The method is simple, rapid, accurate and reliable. It can be applied to control the quality of anthraquinones in Dabaidu capsules.
关 键 词:一测多评 相对校正因子 大败毒胶囊 蒽醌 高效液相色谱法
分 类 号:R917[医药卫生—药物分析学]
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