一種固精補元氣中藥丸摻加Acetaminophen, Piroxicam, Ethoxybenzamide, Hydrochlorothiazide, Chlorzoxazone, Caffeine及Nicotinamide西藥成分之分析與定量研究   全文下載

Quantitative Analysis of Acetaminophen, Ethoxybenzamide, Piroxicam, Hydrochlorothiazide, Caffeine, Chlorzoxazone and Nicotinamide Illegally Adulterated in Chinese Medicinal Pills

來自某廟宇供應香客之固精補元氣中藥丸，經薄層層析法以氯仿：乙醇（9：1, v／v）及乙酸乙脂：甲醇：氯水（8：1：1, v／v）雙向垂直展開後，再以紫外光分光光度計篩檢檢出acetaminophen, piroxicam, ethoxybenzamide, chlorzoxazone, hydrochlorothiazide, caffeine及nicotinamide七種西藥成分。進一步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1%v／v triethylamine - 1 %v／v phosphoric acid buffer（A）, acetonitrile（B）及methanol（C）三種溶媒系，A、B及C以不同之混合比例作梯度沖提，最初60分鐘以90：5：5線性梯度轉變成40：30：30比例沖提，第60-70分鐘再線性梯度轉變回復成90：5：5 比例沖提，以fenbufen為內部標準品，流速1.0 ml／min，檢測波長260nm，注入量10μl。各檢測成分之檢量線，其線性關係（r=0.9997 - 0.9999）良好；其再現性之探討，採一固定已知濃度之混合標準品溶液進行同日內及異日間之測試，其同日內及異日間之相對標準偏差分別為在0.6～3%及1.0～4.6%之間，再現性尚可接受。至於回收率分別為acetaminophen 98.5～104.7%, piroxicam 99.5～104.2%, ethoxybenzamide 97.2～108.0%, hydrochlorothiazide 97.0～118.0%, caffeine 93.3～102.5%, chlorzoxazone 96.0～105.3%及nicotinamide 96.0～103.0%，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acetaminophen 78mg, piroxicam 16mg, ethoxybenzamide 30mg, hydrochlorothiazide 4mg, caffeine 30mg, chlorzoxazone 41mg及nicotinamide 16mg。"

A traditional Chinese medicine, which was supplied as pills by a temple and used as Ch'i tonic, was obtained for testing 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 acetaminophen, piroxicam, hydrochlorothiazide, caffeine, ethoxybenzamide, chlorzoxazone and nicotinamide in the pills. In quantitative analysis, a reversed-phase HPLC method has been established for simultaneous determination of the seven chemical drugs. The analysis of the simple extract was performed on a Cosmosil 5C18AR column (4.6 x 150mm) by a linear gradient elution with 1%triethylamine--1% phosphoric acid buffer, acetonitrile and methanoi(0 min, 90:5:5; 60min, 40:30:30; 70min,90:5:5) as the mobile phase at I ml/min and with fenbufen as an internal standard. The monitor was set at 260nm. System suitability tests showed that the established method was quite suitable for the determination of the adulterants in pills. By using this method, 78mg of acetaminophen, 16mg of piroxicam, 30mg of caffeine, 30mg of ethoxybenzamide, 41 mg of chlorzoxazone, 4mg of hydrochlorothiazide and 16mg of nicotinamide, were found in each pill of the sample.