逆相離子對高效液相層析法同時測定複方中藥中的鹽酸溴克辛和黃芩苷   全文下載

Simultaneous Determination of Bromhexine HCl and Baicalin in Chinese Compound Medicine by a Reversed-Phase Ion-Pair HPLC

本文首次建立了同時測定複方咳喘靈膠囊中鹽酸溴克辛（brornhexine HCl，BHH）和黃芩?（baicalin）的逆相離子對高效液相層析法。探討了四丁基溴化銨（TBA）的濃度、離子對試劑的種類、三乙胺以及有機溶劑的含量對兩種分析物滯留時間的影響。選擇含有0.7 mmol L-1 TBA 的乙?／水／磷酸／三乙胺 （22／78／0.1／0.1，v／v／v／v）移動相在波長225 nm 分離檢測黃芩?和BHH，結果顯示黃芩?和BHH的波峰分別在21min和27min出現，分離度較大，峰形良好，且不受空白對照樣品的干擾。在上述優化的條件下，BHH線性範圍為0.2~15.0μg mL-1，最低檢測限量是0.1 μg mL-1。黃芩?線性範圍為0.1~12.0μg mL-1，最低檢測限量是0.05μg mL-1。平均回收率分別為97.7% （BHH）、99.1% （黃芩?）。結果顯示該方法簡便、通用、快速、準確，可以作為複方中藥含此二類成分藥物的品質管制的檢驗方法。

In this article, a reversed-phase ion-pair high-performance liquid chromatography (HPLC) method was established for simultaneous separation and quantitative analysis of bromhexine HCl (BHH) and baicalin in Chinese Ke-Chuan-Ling compound capsule. The influence of the mobile phase composition on the retention of the analytes was investigated. The optimal determination conditions consisted of acetonitrile/water/phosphoric acid/triethylamine (22/78/0.1/0.1, v/v/v/v) mobile phase with the addition of tetra-n-butylammonium bromide (TBA) (0.7 mmol L-1, terminal concentration) as pairing ion, and a detection wavelength at 225 nm. In this case, baicalin and bromhexine HCl were eluted at 21 min and 27 min respectively and were separated successfully from other ingredients. Excellent linear relationship between the peak area and concentration was obtained in the range of 0.2~15.0 μg mL-1 for bromhexine HCl and 0.1~12.0 μg mL-1 for baicalin. The limit of detection of BHH was 0.1 μg mL-1 and it was 0.05 μg mL-1 for baicalin. The average recoveries of bromhexine HCl and baicalin were 97.7% and 99.1%, respectively. From the results it can be concluded that this method is simple, versatile, and reliable for the quality control of Chinese traditional medicines containing baicalin and/or bromhexine HCl. 本文首次建立了同時測定複方咳喘靈膠囊中鹽酸溴克辛（brornhexine HCl，BHH）和黃芩苷（baicalin）的逆相離子對高效液相層析法。探討了四丁基溴化銨（TBA）的濃度、離子對試劑的種類、三乙胺以及有機溶劑的含量對兩種分析物滯留時間的影響。選擇含有0.7 mmol L-1 TBA 的乙腈／水／磷酸／三乙胺 （22／78／0.1／0.1，v／v／v／v）移動相在波長225 nm 分離檢測黃芩苷和BHH，結果顯示黃芩苷和BHH的波峰分別在21min和27min出現，分離度較大，峰形良好，且不受空白對照樣品的干擾。在上述優化的條件下，BHH線性範圍為0.2～15.0μg mL-1，最低檢測限量是0.1 μg mL-1。黃芩苷線性範圍為0.1～12.0μg mL-1，最低檢測限量是0.05μg mL-1。平均回收率分別為97.7% （BHH）、99.1% （黃芩苷）。結果顯示該方法簡便、通用、快速、準確，可以作為複方中藥含此二類成分藥物的品質管制的檢驗方法。