- 期刊
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
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.
並列摘要
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.