以高效液相層析法分析藥物中之泛酸鈣及其穩定性測試   全文下載

Liquid Chromatographic Method for Determination of Calcium Pantothenate Preparations and Related Stability Studies

本研究的目的在於探討一個適當的高效液相色層分析條件，以檢測藥品中之泛酸鈣的含量。實驗以Alltima C18的管柱，磷酸二氫鉀與乙?溶液（以磷酸調整pH = 2.5）為移動相；結果顯示移動相溶液於1.0 mL／min的流速下可將泛酸鈣與其他之水溶性維生素分離，且於204 nm的紫外線吸收光譜下泛酸鈣有較大的吸收峰。又以ampicillin作為內標準品，泛酸鈣與amplcillin之吸收光譜出現的時間分別約為5.3及6.5分鐘。泛酸鈣的濃度為10-50 μg／mL時吸收光譜中泛酸鈣與ampicillin波峰高度的比值成一線性相關（r = 0.9999）。十二種市售商品標準添加之回收率大於98.96%；而同日間的相對相對標準差介於0.1-0.9%，異日間的相對相對標準差則介於0.1-0.7%。此外，將含有泛酸鈣的原料藥以所發展的HPLC法與USP微生物分析法定量泛酸鈣的含量，並以paired t-test做一配對比較，結果顯示在95%的信賴區間下兩方法間並無顯著差異。此結果顯示本研究的方法可代替USP微生物分析法定量藥物中泛酸鈣的含量，且更為快速、穩定並具再現性。

This report describes a fast, simple and reliable HPLC method for the assay and quantitative determination of calcium pantothenate in commercial products. The samples were analyzed on a C18 column with the mobile phase of acetonitrile and potassium dihydrogen phosphate solution (adjusted pH = 2.5 with phosphoric acid) at a flow rate of 1.0 mL/min and UV absorbance detection at 204 nm. Ampicillin was used as an internal standard. The retention times of calcium pantothenate and ampicillin were 5.3 and 6.5 min, respectively. An equation was presented for linear relationship between peak height ratios of calcium pantothenate to ampicillin and the calcium pantothenate concentration over a range of 10-50 μg/mL (r = 0.9999). Standard addition recoveries were greater than 98.96% with twelve commercial products. The relative standard deviations were between 0.1 and 0.9% in inter-day assays, 0.1 and 0.7% in intra-day assays. The results obtained from the HPLC assay method which we developed and the microbiological assay of USP were paired at 95% confidence level. There were no significant differences between these two methods. The proposed HPLC method was a suitable substitute for microbiological method for quantitative assays of calcium pantothenate in commercial products. 本研究的目的在於探討一個適當的高效液相色層分析條件，以檢測藥品中之泛酸鈣的含量。實驗以Alltima C18的管柱，磷酸二氫鉀與乙腈溶液（以磷酸調整pH = 2.5）為移動相；結果顯示移動相溶液於1.0 mL／min的流速下可將泛酸鈣與其他之水溶性維生素分離，且於204 nm的紫外線吸收光譜下泛酸鈣有較大的吸收峰。又以ampicillin作為內標準品，泛酸鈣與amplcillin之吸收光譜出現的時間分別約為5.3及6.5分鐘。泛酸鈣的濃度為10-50 μg／mL時吸收光譜中泛酸鈣與ampicillin波峰高度的比值成一線性相關（r = 0.9999）。十二種市售商品標準添加之回收率大於98.96%；而同日間的相對相對標準差介於0.1-0.9%，異日間的相對相對標準差則介於0.1-0.7%。此外，將含有泛酸鈣的原料藥以所發展的HPLC法與USP微生物分析法定量泛酸鈣的含量，並以paired t-test做一配對比較，結果顯示在95%的信賴區間下兩方法間並無顯著差異。此結果顯示本研究的方法可代替USP微生物分析法定量藥物中泛酸鈣的含量，且更為快速、穩定並具再現性。