摘要
目的采用HPLC法和旋光度法测定布洛芬注射液中精氨酸的含量,并从中选择适宜的方法。方法 HPLC法采用Kromasil NH2色谱柱(250 mm×4.6 mm,5μm),以乙腈-磷酸氢二钾溶液(取磷酸氢二钾4.56 g,加水1 000 mL使溶解,磷酸溶液调节pH值至3.5)(体积比57∶43)为流动相,流速1.0 mL.min-1,检测波长214 nm,柱温30℃;旋光度法照《中华人民共和国药典》2010版附录ⅥE旋光度测定法项下的方法操作直接测定布洛芬注射液的旋光度。结果 HPLC法:主药布洛芬与精氨酸分离度良好,精氨酸质量浓度在0.078～0.780 g.L-1内与峰面积呈良好的线性关系,回归方程为A=8.016×104ρ-1.039×103(r=0.999 8,n=6),方法的最低检测限为150 ng,平均回收率为99.72%,RSD为0.98%(n=9);旋光度法:主药布洛芬不干扰精氨酸测定,溶液质量浓度在63.0101.0 g.L-1内旋光度线性关系良好,回归方程为α=104.5ρ-3.039(r=0.999 7,n=6),平均回收率为99.10%,RSD为0.58%(n=9)。结论两种方法均适用于布洛芬注射液中精氨酸的含量测定,可有效测定精氨酸的含量,测定结果也比较一致。相比较而言,旋光度测定法简便快速。
Objective To establish an effective and reliable determination method for determination of the content of arginine in ibuprofen injection through comparing HPLC and optical rotation photometry methods.Methods Kromasil NH2 column（250 mm×4.6 mm,5 μm）was used in HPLC method with the mobile phase consisted of acetonitrile-20 mmol · L-1 dipotassium hydrogenphosphate solution（V∶ V=57∶ 43）.The flow rate of mobile phase was 1.0 mL · min-1,the UV detection wavelength was set at 214 nm and the column temperature was at 30 ℃;Optical rotation of ibuprofen injection was determined according to appendixes Ⅵ E of Chinese Pharmacopoeia 2010 edition.Results HPLC method：The calibration curve was linear within the range of 0.078 to 0.780 g · L-1（A=8.016×104ρ-1.039×103,r=0.999 8,n=6）;the lowest limit determination was 150 ng（S/N=3）.The mean recoveries of high,middle and low concentration were 99.72%（n=9,RSD=0.45%）.Optical rotation photometry method：The calibration curve was linear within the range of 63.0 to 101.0 g · L-1（α=104.5ρ-3.039,r=0.999 7,n=6）;The mean recoveries of high,middle and low concentration were 99.10%（n=9,RSD=0.58%）.Conclusions Two methods are accurate and suitable for determination of the content of arginine.The optical rotation photometry method is simple.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2013年第6期442-445,477,共5页
Journal of Shenyang Pharmaceutical University
基金
卫生行业科研专项资助项目(200902008)
国家“十二五”重大新药创制科技重大专项资助项目(2011ZX09203-001-16)
