枸橼酸莫沙必利原料药及制剂中有关物质测定的液相色谱法的建立与验证
Development and validation of a liquid chromatographic method for determination of related-substances of mosapride citrate in bulk drugs and pharmaceuticals.
作者信息
Nageswara Rao R, Nagaraju D, Alvi S N, Bhirud S B
机构信息
HPLC/UV Group, Division of Analytical Chemistry, Discovery Laboratory Indian Institute of Chemical Technology, Hyderabad 50 0007, India.
出版信息
J Pharm Biomed Anal. 2004 Nov 19;36(4):759-67. doi: 10.1016/j.jpba.2004.08.004.
An isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method for determination and evaluation of purity of mosapride citrate in bulk drugs and pharmaceuticals has been developed using Waters Symmetry C(18) column with acetonitrile:0.024 M orthophosphoric acid (28:72, v/v) adjusted to pH 3.0 with triethylamine and photodiode array detector set at 276 nm. The method is simple, rapid, selective and capable of detecting all process related impurities at trace levels in the finished products with detection limits ranging in between 0.2 x 10(-8)g and 6.4 x 10(-8)g. The method has been validated with respect to accuracy, precision, linearity, ruggedness, and limit of detection and quantification. The linearity range was 125-1000 microg/ml. The percentage recoveries from pharmaceutical dosages were ranged from 95.53 to 100.7. The method was found to be suitable not only for monitoring the reactions during the process development but also quality assurance of mosapride citrate.
已开发出一种等度反相高效液相色谱（RP - HPLC）法，用于测定和评估原料药及制剂中枸橼酸莫沙必利的纯度。该方法采用沃特世Symmetry C(18) 色谱柱，以乙腈∶0.024 M正磷酸（28∶72，v/v）为流动相，用三乙胺调节pH值至3.0，采用光电二极管阵列检测器，检测波长为276 nm。该方法简便、快速、具有选择性，能够检测成品中痕量的所有工艺相关杂质，检测限在0.2×10(-8)g至6.4×10(-8)g之间。该方法在准确性、精密度、线性、耐用性以及检测限和定量限方面均已得到验证。线性范围为125 - 1000μg/ml。药物制剂的回收率在95.53%至100.7%之间。结果表明，该方法不仅适用于工艺开发过程中的反应监测，也适用于枸橼酸莫沙必利的质量保证。
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