盐酸普拉克索缓释微丸胶囊的制备及有关物质检测  

Preparation of Pramipexole Dihydrochloride Sustained-release Pellets Capsules and Related Substances Determination

作　　者：戈文兰[1] 张根元[1] 

机构地区：[1]江苏省药物研究所有限公司,南京210009

出　　处：《中国药房》2016年第31期4433-4435,共3页China Pharmacy

摘　　要：目的：制备盐酸普拉克索缓释微丸胶囊,建立其有关物质的检测方法。方法：采用流化床空气悬浮包衣法制备载药丸芯,以乙基纤维素水分散体（Surelease）进行包衣,制成盐酸普拉克索缓释微丸,装入胶囊即可。采用高效液相色谱（HPLC）法检测缓释微丸中有关物质,色谱柱为Capcell PAK MG-ⅡC18（150 mm×4.6 mm,5μm）;梯度洗脱,流动相A为甲酸铵缓冲液（p H 5.0）,流动相B为甲醇;流速为1.0 ml/min;二极管阵列检测器,检测波长为240、262、326 nm;进样量为80μl。结果：该色谱条件下,盐酸普拉克索能与7种有关物质完全分离,且空白辅料不干扰测定,7种有关物质检测质量浓度的线性范围均为0.2-2μg/ml（r〉0.999 0）,检测限为0.5-1.8 ng,定量限为1.7-5.9 ng,平均回收率为98.93%-102.0%（RSD为1.90%-0.24%,n=9）,精密度和稳定性试验的RSD均小于1.0%（n=5）。所制得的盐酸普拉克索缓释微丸胶囊中仅检测出1种有关物质。结论：成功制得盐酸普拉克索缓释微丸胶囊;所建立的HPLC法可用于其有关物质的检测。OBJECTIVE： To prepare Pramipexole dihydrochloride sustained-release pellets capsules and to establish a method for the determination of related substances. METHODS： Drug loaded core was prepared by fluid bed air suspension coating method, and pramipexole dihydroehloride pellets were prepared using Surelease~ as coating materials and put into capsules. HPLC method was used to determine related substance in sustained-release pellets; the determination was performed on Capcell PAK MG- II C18 column （150 mm×4.6 mm, 5 μm） with mobile phase A consisted of ammonium formate buffer solution （pH 5.0） and mobile phase B consisted of methanol for gradient elution at flow rate of 1.0 ml/min; diode array detector was used with detection wavelength of 240, 262, 326 nm and injection volume of 80 μl. RESULTS： Pramipexole dihydrochloride and 7 kinds of related substances were separated by the established HPLC conditions. The blank excipient did not interfere with the assay of the related substances. The linear ranges of 7 related substances were 0.2-2 μg/ml （r〉0.999 0） ; the limit of detection ranged 0.5-1.8 ng, and the limit of quantitation ranged 1.7-5.9 ng; average recovery ranged 98.93%-102.0% （RSD were 1.90%-0.24%,n=9）. RSD of precision and stability test were all lower than 1.0% （n=5）. Only one related substance was found in prepared Pramipexole dihydrochloride pellets capsules. CONCLUSIONS： Pramipexole dihydrochloride pellets capsules are prepared successfully. Established HPLC method can be used for the determination of its related substances.

关 键 词：盐酸普拉克索 缓释微丸 胶囊 制备 高效液相色谱法 有关物质 检测 

分 类 号：R943[医药卫生—药剂学]