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題 名 | 市售大陸中藥標示壯陽功能產品之調查檢驗=Determination by Liquid Chromatography-tandem Mass Spectrometry on Sildenafil and Tadalafil Adulterated in Traditional Chinese Medicines from China |
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作 者 | 曾木全; 劉宜祝; 林哲輝; | 書刊名 | 藥物食品檢驗局調查研究年報 |
卷 期 | 23 民94.09 |
頁 次 | 頁136-148 |
分類號 | 412.36 |
關鍵詞 | 液相層析串聯式質譜分析法; MRM定量分析法; 大陸壯陽類中藥; 中藥製劑摻加西藥成分; Sildenafil; Tadalafil; Pirenzepine; LC/MS/MS; Chinese medicines; Treatment of male erectile dysfunction; Sildenafil citrate; ESI; MRM; Daughter ion scan; |
語 文 | 中文(Chinese) |
中文摘要 | 行政院衛生署藥物食品檢驗局自91 年1 月起至92 年3 月止,受理大陸產製中藥檢驗案件中,總共有22 件次計17 種品目之大陸壯陽類中藥檢出西藥成分,其中15 種檢出sildenafil,2 種檢出tadalafil,其中安徽三體醫藥保健公司產製之藥品有三種品目,其餘隸屬於12家不同之廠家。 檢體篩檢方法為檢體粉末經以50 %甲醇萃取、稀釋及過濾,取 濾液直接注入液相層析串聯式質譜儀(LC/MS/MS)分別進行正離子電灑法(ESI+)之m/z 475 及m/z 390 子代離子掃描,獲得之子代離子質譜圖(Daughter ion spectrum)與本局自建液相層析質譜資料圖庫(NLFD3/LM library)比對,初步快速篩檢是否含上述兩成分,若疑似檢出者,須再經HPLC 分離及串聯式質譜儀分析。儀器之分析條件:分離管柱均為Cosmosil 5C18-AR, 4.6 150mm。移動相溶媒系,sildenafil 為甲醇:乙腈:1 %醋酸(25:17:58);tadalafil 為乙腈:水: 1 %醋酸(50 : 45: 5);流速:0.5 mL/min(1:1 分流),毛細管電壓:3 kV;進樣圓錐口電壓及碰撞能量設定:sildenafil 為80 V 及25 eV;而tadalafil 為60 V 及18 eV;離子源溫度:120℃;溶媒揮散溫度:300℃,配合附光二極體陣列檢出器(photodiode array)檢測之結果檢品溶液離子峰滯留時間、紫外光光譜圖及質譜圖與對照標準品比對結果均相符,確認檢品摻加sildenafil 及tadalafil 西藥成分。 為探討檢體中所含相當於sildenafil citrate 及tadalafil 之量而配製系列對照標準品溶液,以pirenzepine 作為內部標準品,分別選定親代及子代離子(m/z 475.4>100.2,m/z 390.2>268.0)作多重離子裂解監控(MRM, Multiple Reaction Monitoring)定量分析並製作檢量線,其線性關係γ值分別為0.9993 及0.9985。 |
英文摘要 | The commercial VIAGRA(r) products have arisen a phenomenon. As aresult, many off Chinese medicines and food supplements claimed to have treatment effects on male erectile dysfunction. From January 2002 to March 2003, Bureau of Food and Drug Agency (BFDA) received 22 samples in 17 different traded names that were marketed in China. All of the samples were found illegally adulterated with sildenafil or tadalafil. Among the 17 different branded samples, 3 were manufactured by An Wei San Tee Medicinal Health Company(安徽三體醫藥保健公司), the rest were manufactured by different companies. Sample powder was extracted with 50% methanol and analyzed by LC/MS/MS, detected by photodiode array and tandem mass detector with positive electron spray ionization (ESI+) method. The testing conditions were set as following: Column: Cosmosil 5C18-AR,Mobile phase:methanol:acetonitrile:1% acetic acid (25:17:58) for sildenafil analysis; and acetonitrile:water:1% acetic acid(50 : 45: 5)for tadalafil analysis; Flow rate: 0.5mL /min (1:1 split); Voltage of capillary tube:3KV; Voltage of sample cone and collision energy were 80V/25eV and 60V/18eV for sildenafil and tadalafil respectively. The source temperature was set on 120oC, and the solvent desolvation temperature on 350oC. The daughter ion scan was set at m/z 475 for sildenafil and m/z 390 for tadalafil to obtain a daughter ion spectrum. The result were then compared with the data library (NLFD3/LM) that was set up by the lab. The existence of the adulterants were confirmedwhen the ion peaks retention time of samples, as well as the UV and mass spectrum patterns of the samples matched with the sildenafil and tadalafil data as recorded in the library. The quantity of sildenafil and tadalafil were calculated by calibration curves. Both pair of parent and daughter ion (m/z 475>100 and m/z 390>268) were chosen and multiple reaction monitoring (MRM) was performed. The results were then referred to the calibration curves (γ2=0.9993 and 0.9985) to determine the amount of sildenafil and tadalafil in samples. |
本系統中英文摘要資訊取自各篇刊載內容。