治療心臟病與排尿酸用之中藥丸中摻加Caffeine, Diazepam, Chlorzoxazone, Ethoxybenzamide及Indomethacin西藥成分之分析與定量研究   全文下載

Quantitative Analysis of Caffeine, Ethoxybenzamide, Chlorzoxazone, Diazepam and Indomethacine Illegally Adulterated in Chinese Medical Pills

來自消費者自稱用於治療心臟病、排尿酸之中藥丸，經薄層層析法，以氯仿：乙醇（9:1, v／v） 及乙酸乙酯：甲醇：氨水（8:1:1, v／v）雙向展開後，再以紫外光分光光度計篩檢檢出indomethacin, caffeine, ethoxybenzamide, chlorzoxazone及diazepam五種西藥成分。續以逆相高效液相層析法探討定量，採Cosmosil 5C18-AR層析管柱（4.6×150 mm），移動相為0.05M磷酸二氫鉀-0.1%甲酸緩衝溶液（A）及甲醇（B）二種溶媒系，A及B以不同之混合比例作線性梯度沖提，最初30分鐘以60:40遞變成40:60比例沖提，第30～60分鐘則維持40:60比例沖提，第60～75分鐘線性梯度回復成60:40比例沖提，以propylparaben為內部標準品，流速每分鐘0.7ml，檢測波長230nm，注入量10μl，各檢測成分之檢量線，其線性關係（r=0.9995～0.9999）良好；有關再現性之探討，採一固定已知濃度之混合標準品溶液進行同日內及其日間之測試，其同日內及其日間之相對標準偏差分別在0.7～2.8%及1.5～3.0%之間，顯示再現性亦佳。至於添加回收率分別為indomethacin 96.0～109.0%, caffeine 96.7～103.4%, ethoxybenzamide 98.7～107.6%, chlorzoxazone 99.5～106.4%及diazepam96.0～103.0%顯示準確性均良好。經定量結果，每丸中各西藥成分之平均含量分別為indomethacin 9.3mg, ethoxybenzamide 71.4 mg, caffeine 30.8 mg, chlorzoxazone 35.7 mg及diazepam 0.6 mg。 A traditional Chinese medicine, which was brought by a consumer for treating heart disease and uricosuria, was obtained and tested the illegal adulteration with chemical drugs. In the qualitative analysis, two-dimensional TLC, with chloroform: ethanol (9: 1, v/v) and ethyl acetate: methanol: ammonia water (8:1:1, v/v) as the solvent systems, established the presence of caffeine, indomethacin, ethoxybenzamide, chlorzoxazone and diazepam in the pills. For quantitative analysis, a reversed-phase HPLC method was established for simultaneous determination of the five chemical drugs. The analysis of the sample extract was performed on a Cosmosil 5C18-AR column (4.6x150mm) by a linear gradient elution with the mobile phase of 0.05 M KH2 P04-0.1% formic acid buffer and methanol, programmed from 60:40, v/v, to 40:60, v/v, for 30 min, with 30 min hold and then 60:40, v/v, for the subsequent 15 min, at a flow rate of 0.7 ml/min and with propylparaben as an internal standard. The monitor wavelength was set at 230 nm. System suitability tests showed that the established method was quite suitable for the determination of the adulterants in the pills. By using this method, 30.8mg of caffeine, 71.4 mg of ethoxybenzamide, 35.7 mg of chlorzoxazone, 0.6 mg of diazepam and 9.3 mg of indomethacin, were found in each pill of the sample."

A traditional Chinese medicine, which was brought by a consumer for treating heart disease and uricosuria, was obtained and tested the illegal adulteration with chemical drugs. In the qualitative analysis, two-dimensional TLC, with chloroform: ethanol (9: 1, v/v) and ethyl acetate: methanol: ammonia water (8:1:1, v/v) as the solvent systems, established the presence of caffeine, indomethacin, ethoxybenzamide, chlorzoxazone and diazepam in the pills. For quantitative analysis, a reversed-phase HPLC method was established for simultaneous determination of the five chemical drugs. The analysis of the sample extract was performed on a Cosmosil 5C18-AR column (4.6x150mm) by a linear gradient elution with the mobile phase of 0.05 M KH2 P04-0.1% formic acid buffer and methanol, programmed from 60:40, v/v, to 40:60, v/v, for 30 min, with 30 min hold and then 60:40, v/v, for the subsequent 15 min, at a flow rate of 0.7 ml/min and with propylparaben as an internal standard. The monitor wavelength was set at 230 nm. System suitability tests showed that the established method was quite suitable for the determination of the adulterants in the pills. By using this method, 30.8mg of caffeine, 71.4 mg of ethoxybenzamide, 35.7 mg of chlorzoxazone, 0.6 mg of diazepam and 9.3 mg of indomethacin, were found in each pill of the sample.