HPLC波长切换法同时测定三黄胶囊中7种成分的含量  

Simultaneous Determination of Contents of Seven Components in Sanhuang Capsule by HPLC Wavelength Switching Method

作　　者：王雷 于荣 Wang Lei Yu Rong(Cardiovascular Hospital of Shanxi, Taiyuan 030024, Chin)

机构地区：[1]山西省心血管病医院,太原030024

出　　处：《中国药事》2016年第11期1100-1106,共7页Chinese Pharmaceutical Affairs

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.

关 键 词：三黄胶囊 高效液相色谱 波长切换法 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 

分 类 号：R284.1[医药卫生—中药学] R927.2[医药卫生—中医学]