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机构地区:[1]广东药学院,广州510224
出 处:《中国药房》2014年第12期1118-1121,共4页China Pharmacy
基 金:广东省自然科学基金资助项目(No.5002841)
摘 要:目的:建立同时测定清肺抑火丸中5种蒽醌类成分大黄素、芦荟大黄素、大黄酸、大黄酚、大黄素甲醚含量的方法。方法:采用毛细管电泳法,以对乙酰氨基酚为内标。毛细管柱为未涂层弹性融硅石英毛细管柱,运行缓冲液为25mmol/L硼砂溶液+20mmol/L十二烷基磺酸钠+4mmol/L磺丁基醚.伊环糊精+2%甲醇(pH10.01),分离电压为18kv,进样方式为重力进样10s(高度15cm),检测波长为254nm,温度为25℃,湿度为〈70%。结果:大黄素、芦荟大黄素、大黄酸、大黄酚、大黄素甲醚检测质量浓度分别在5.0~40.0、2.4~19.2、3.6~28.8、11.2~89.9、2.5~20.0μg/ml范围内同各自峰面积与内标峰面积比值呈良好的线性关系(r=0.9980、0.9971、0.9969、0.9985、0.9983);精密度、稳定性、重复性试验的RSD≤2.40%;平均加样回收率分剐为96.6%、99.6%、99.2%、98.2%、98.6%,RSD分别为0.80%、1.32%、2.21%、1.63%、2.02%(n=6)。结论:该方法专属性强,结果准确、可靠,重复性好,可用于清肺抑火丸的质量控制。OBJECTIVE: To establish a method for simultaneous determination of 5 anthraquinones in Qingfei yihuo pills, such as emodin, aloe-emodin, rhein, chrysophanol and physcion. METHODS: Capillary electrophoresis was adopted using paracetamol as internal standard. The separation was performed on a uncoated fused silica capillary. 25 mmol/L Na2B4O7+20 mmol/L SDS +4 mmol/L SBE-β-CD+2% methanol solutionfpll 10.01)was selected as the running buffer. The voltage applied was 18 kV. The sample was injected by gravity (1 0 s, 15cm). The detection wavelength was set at 254 nm. The column temperature was 25 ℃ and humidity was lower than 70%. RESULTS: The linear range of emodin, aloe-emodin, rhein, chrysophanol, physcion were 5.0-40.0 μg/ml(r=0.998 0), 2.4-19.2 μg/ml(r=0.997 1), 3.6-28.8μg/ml(r=0.996 9), 11.2-89.9 μg/ml(r=0.998 5), 2.5-20.0 μg/ml (r=0.998 3) , respectively; RSDs of precision, stability and reproducibility tests were all lower than 2.40%; average recoveries were 96.6% (RSD=0.80%, n=6), 99.6% (RSD=1.32%, n=6), 99.2% (RSD=2.21%, n=6), 98.2% (RSD=1.63%, n=6) and 98.6% (RSD=2.02%, n=6). CONCLUSIONS: The method is proved to be specific, accurate, reliable and reproducible, and can be used for quality control of Qingfei yihuo pills.
关 键 词:毛细管电泳法 清肺抑火丸 大黄素 芦荟大黄素 大黄酸 大黄酚 大黄素甲醚 含量测定
分 类 号:R917[医药卫生—药物分析学]
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