高效液相層析法及化學計量為基礎的分光光度法檢驗 Ramipril 及 Atorvastatin 製劑   全文下載

Validated High-Performance Liquid Chromatographic and Chemometric Based Spectrophotometric Determination of Ramipril and Atorvastatin in Pharmaceutical Dosage Forms

本研究開發一種快速、簡單之逆相高效液相層析法及三種以古典最小平方（CLS）、主成分迴歸（PCR）和部分最小平方（PLS）檢量的分光光度法，可同時檢測ramipril（RAMP）和atorvastatin calcium（ATOR）製劑。高效液相層析法使用Phenomenex-Luna RP C-18管柱（250 × 4.6 mm, 5 mm），移動相為乙?：0.1 M sodium perchlorate（pH 2.5）（70：30，V/V），流量1.5 mL/min，紫外光偵測波長為210 nm。化學檢量法以25個檢體為一組進行實驗，在波長201 – 270 mm（Δλ = 1 nm）零級光譜範圍內，以吸收數據矩陣配合濃度數據矩陣計算其化學成分，數字的計算係使用新R-Software Environment軟體（v. 2.1.1）。方法預估可靠度經各種ICH管制參數確效。化學計量法和層析法之檢測結果，經比較具一致性。實驗室製備的混合物和錠劑產品都能成功地以本研究開發之方法檢測。"

A fast, simple RP-HPLC and three spectrophotometric methods based on classical least squares (CLS), principle component regres-sion (PCR) and partial least squares (PLS) calibrations were developed for simultaneous estimation of ramipril (RAMP) and atorvastatin calcium (ATOR) in formulations. The HPLC assay utilized Phenomenex - Luna RP C-18 (2) 250 × 4.6 mm 5 μm column with mobile phase composition of acetonitrile: 0.1 M sodium perchlorate (pH 2.5) (70 : 30, v/v), and flow rate of 1.5 mL/min with UV detection at 210 nm. Chemometric calibrations were constructed by using absorption data matrix corresponding to concentration data matrix, with measure-ments in the range of 201-270 nm (Δλ = 1 nm) in their zero-order spectra using 25 samples in training set. The chemometric numerical computations were realized using novel R-Software Environment (version 2.1.1). Reliability of predictions was validated for various ICH regulatory parameters. Both the results of proposed chemometric methods and that of proposed chromatographic method were compared and good agreement was found. Laboratory prepared mixtures and commercial tablet formulations were successfully analyzed by the developed methods.