The Study for Adulterant Tonic Component of Tadalafil in Chinese Herbal Medicine and Food
| Autor: | Mei-Li Lin, 林美悧 |
|---|---|
| Rok vydání: | 2005 |
| Druh dokumentu: | 學位論文 ; thesis |
| Popis: | 93 This study focused on the analysis method for adulterant tonic component of tadalafil [the major component of Cialis (commercial name)] in Chinese herbal medicine and food. A simple, reliable, and reproducible high performance liquid chromatography (HPLC) method was used for determination of tadalafil in Chinese herbal medicine and food. The sample was extracted with 95% ethanol. A Supersil ODS column (5 mm, 4.6 × 250 mm) was used as the analytical column. The mobile phase was methanol: water (80:20, v/v). The injection volumn was 10 mL. The flow rate was set at 1.0 mL/min. The detection wavelength was 283 nm. The correlation coefficients of linear calibration curves at both high (100-1000 ppm) and low concentration (10-100 ppm) of tadalafil were greater than 0.999. The recoveries were assessed by spiking 500 mg/g of tadalafil into a commercial matrix. The mean recovery was 109.9% (n = 3), and the standard deviation(SD) is 3.67﹪. The detection limit of the HPLC method is 1.5 ppm for tadalafil. Five solvent systems were used in thin layer chromatography (TLC) for qualitative analyses. There were n-butanol: water: acetic acid = 7:2:1 (v/v); ethyl acetate: ether = 4:1 (v/v); chloroform: ethanol = 9:1 (v/v), chloroform: ethyl acetate = 1:1 (v/v) and ethyl acetate: methanol: ammonia water = 8: 1: 1(v/v). The TLC spot of tadalafil was observed when the plate was exposed at 254 nm. After spraying with H2SO4: ethanol = 1:1 solution and heating, the color of the spot became purple. The maximum absorbance occurred at 283, 221, and 206 nm. A HP-5MS capillary column (crosslinked 5% PH ME siloxane, 0.25 mm i.d. × 30 m length × 0.25 mm df ) was used in a gas chromatography/mass spectrometry system to give the retention time of 38.64 min. and the m/z ratios of 389, 262, and 204. The mass transition of tadalafil fragment was from the m/z ratio of 390.20 to 268.00 by analyzing with liquid chromatography-tandem mass spectrometry。 The qualitative and quantitative methods established in the study provide easy ways for determination of adulteration of tadalafil in traditional Chinese medicine and food. |
| Databáze: | Networked Digital Library of Theses & Dissertations |
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