摘要
目的：建立高效液相色谱波长切换法同时测定三黄胶囊中盐酸小檗碱、黄芩苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚7种成分的含量。方法：采用以十八烷基硅烷键合硅胶为填充剂的色谱柱（4.6 mm×150 mm,5μm）,以甲醇（A）-磷酸盐缓冲液（B）（磷酸氢二钠2.3996 g溶解于1000 m L水中,用磷酸调p H值至3.0）为流动相,梯度洗脱（0～5 min,30%A;5～15 min,30%～60%A;15～35 min,60%～100%A;35～40 min,30%A）;波长：0～10 min,345 nm;10～15 min,280 nm;15～40 min,254 nm;流速为1.0 m L·min-1;柱温30℃;进样量10μL。结果：盐酸小檗碱、黄芩苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的线性范围分别是0.09044～1.809μg（r=0.9994）、0.2828～5.656μg（r=0.9995）、0.05805～1.161μg（r=0.9999）、0.05144～1.028μg（r=0.9999）、0.02034～0.4068μg（r=0.9997）、0.04682～0.9364μg（r=0.9998）、0.02540～0.5080μg（r=0.9990）;平均加样回收率（n=6）分别为97.76%、97.09%、98.06%、99.42%、99.28%、96.94%、97.73%,RSD分别为1.67%、1.82%、1.46%、0.89%、1.17%、1.03%、1.59%。结论：该方法操作简单,重复性好,可用于三黄胶囊的质量控制。
Objective： To develop an HPLC method for simultaneous determination of 7 components in Sanhuang Capsule, including berberine hydrochloride, baicalin, aloe-emodin, emodin, rhein, chrysophanol, and physcion. Methods： The Agilent ZORBAX Eclipse XDB-C18（4.6 mm×150 mm, 5 μm） column was used; the mobile phase was methanol（A）-phosphate buffer solution（B）（containing 2.3996 g disodium hydrogenphosphate in 1000 m L water and adjusting p H to 3.0 with phosphoric acid） with gradient elution（0-5 min, 30% A; 5-15 min, 30%-60% A; 15-35 min, 60%-100% A; 35-40 min, 30% A） at a flow rate of 1.0 m L·min-1, and the detection wavelengths were： 0-10 min, 345 nm; 10-15 min, 280 nm; 15-40 min, 254 nm, the column temperature was 30 ℃. Results： The linear ranges of berberine hydrochloride, baicalin, aloe-emodin, emodin, rhein, chrysophanol, physcion were 0.09044-1.809 μg（r=0.9994）, 0.2828-5.656 μg（r=0.9995）, 0.05805-1.161 μg（r=0.9999）, 0.05144-1.028 μg（r=0.9999）, 0.02034-0.4068 μg（r=0.9997）, 0.04682-0.9364 μg（r=0.9998）, 0.02540-0.5080 μg（r=0.9990）; the average recoveries（n=6） were 97.76%, 97.09%, 98.06%, 99.42%, 99.28%, 96.94%, 97.73%, and the RSDs were 1.67%, 1.82%, 1.46%, 0.89%, 1.17%, 1.03%, 1.59%, respectively. Conclusion： The method is easy, accurate and reproducible. It can be used for the quality control of Sanhuang Capsule.
作者
王雷
于荣
Wang Lei Yu Rong(Cardiovascular Hospital of Shanxi, Taiyuan 030024, Chin)
出处
《中国药事》
CAS
2016年第11期1100-1106,共7页
Chinese Pharmaceutical Affairs
