摘要
目的建立使用HPLC测定盐酸雷莫司琼原料中有关物质和右旋体的检测和控制方法。方法采用Diamonsil C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.05 mol.L-1磷酸盐缓冲液(pH5.2)(30∶70)为流动相,流速为1.0 mL.min-1,检测波长为210 nm,测定盐酸雷莫司琼原料中有关物质;采用CHIRAL NEA-R(4.6 mm×250 mm,5μm)手性柱,以乙腈-0.05mol.L-1磷酸二氢钾溶液(pH5.2)(50∶50)为流动相,流速为1.0 mL.min-1,检测波长为306 nm,检查样品中右旋体的含量。结果盐酸雷莫司琼与合成反应中的4个重要中间体,能够得到有效分离,控制总杂质不超过1.0%。S-(+)和R-(-)盐酸雷莫司琼的保留时间分别为10.2和8.9 min,分离度大于2.5。结论上述方法准确、简便、专属,适用于盐酸雷莫司琼中有关物质及右旋体检查。
OBJECTIVE To develop a HPLC method for the determination of related substances and S-（ ＋ ） enantiomer in ramosetron hydrochloride. METHODS A separation for its related substances was performed on a Diamonsil Cis column （4. 6 mm × 250 mm,5 μm）, and mobile phase was acetonitrile-0. 05 mol · L ^-1 phosphate buffer （pH 5.2） （30： 70） with a flow rate of 1.0 mol · L ^-1. The detection wavelength was 210 nm. The other separation for S-（ ＋ ） enantiomer was performed on a CHIRAL NEA-R column （4. 6 mm x250 ram,5 μm） , and mobile phase consisted of acetonitrile-0. 05 tool · L-I phosphate buffer （pH 5.2） （50：50） with a flow rate of 1.0 mL · min ^-1. The detection wavelength was 306 nm. RESULTS A satisfactory separation condition for the four related impurities and the sample was obtained. The total impurities were not more than 1.0%. The retention times for the S-（ ＋ ） and R- （ - ） ramosetron hydrochloride were 8.9 and 10. 2 min respectively with a resolution factor of more than 2.5. CONCLUSION The methods are simple, fast, accurate and specific,and can be used in the determination of related substances and S-（ ＋ ） enantiomer in ramosetron hydrochloride.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2007年第5期386-388,共3页
Chinese Pharmaceutical Journal
