以液相層析儀及分光光度計檢測乳霜中 Diflucortolone Valerate 及Chlorquinaldol   全文下載

Liquid Chromatographic and Spectrophotometric Determination of Diflucortolone Valerate and Chlorquinaldol in Creams

本研究利用新式逆相高效液相層析（HPlC）法及分光光度法同時檢測乳霜中diflucortolone valerate（diF）及chlorquinaldol（CHl）。等梯度系統條件為：aCER C18分析管柱；流動相組成為甲醇/磷酸緩衝溶液（pH 5.5，0.1 m）（95:5，v/v）；流速為1.0 ml/min；紫外光檢測波長：220 nm。內標準品為ephedrine hydrochloride。在分光光度法中，主成分迴歸（PCr）被應用為化學計量工具。其中，各合成藥品混合物溶於甲醇/水（3:1），以製備不同濃度樣品。在零級光譜波長範圍230-348 nm間，取適當波長間隔2 nm，計算60個波的吸收值，以得到diF及CHl各濃度相對的吸收值。lC法所得到的diE及CHl之線性範圍分別為2.40-300 μg/ml及0.72-240 μg/ml；PCr法所得到的diE及CHl之線性範圍分別為0.88-3.0 μg/ml及1.0-11.2 μg/ml。本方法的準確性、精確性及線性範圍已被評估，並藉由分析內含主題藥物之合成混合物而進行確效。這兩種方法已成功地應用於兩類含藥乳霜之製備。

A new reversed phase high pressure liquid chromatography and a spectrophotometric method are proposed for the simultaneous determination of diflucortolone valerate (DIF) and chlorquinaldol (CHL) in creams. An isocratic system consisted of an ACE® C18 analytical column and a mobile phase composed of methanol/phosphate buffer (pH 5.5, 0.1 M) (95:5, v/v) at a flow rate 1.0 mL/min was used for the optimal chromatographic separation using UV detection at 220 nm. Ephedrine hydrochloride was used as internal standard. Principal component regression (PCR) was used as the chemometric technique in spectrophotometry. In this technique, the concentration data matrix was prepared by using the synthetic mixtures containing these drugs in methanol/water (3:1). The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbances at 60 wavelengths in the range of 230-348 nm with appropriate interval Δλ of 2 nm for DIF and CHL in the zero-order spectra for the binary combinations. The linear ranges were found 2.40-300 μg/mL for DIF, 0.72-240 μg/mL for CHL for LC method, and 0.88-3.0 μg/mL for DIF and 1.0-11.2 μg/mL for CHL for PCR method. The accuracy, precision and the linear ranges of the methods have been evaluated and they have been validated by analyzing synthetic mixtures containing the title drugs. These two methods were successfully applied to two pharmaceutical cream preparations and the results were compared with each other.