篇名 | 應用氣相層析質譜儀及高效液相層析儀分析中藥製劑摻加Phenformin西藥成分之研究 |
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卷期 | 9:3 |
並列篇名 | Detection and Determination of Phenformin in Chinese Medicinal Capsules by GC-MS and HPLC |
作者 | 林美智 、 林哲輝 、 溫國慶 |
頁次 | 139-144 |
關鍵字 | 中藥摻加西藥 、 氣相層析質譜儀 、 高效液相層析法 、 Phenformin 、 Traditional Chinese medicine 、 GC-MS 、 High performance liquid chromatography 、 MEDLINE 、 Scopus 、 SCIE |
出刊日期 | 200109 |
治療糖尿病之phenformin (芬法敏)由於使用後會造成乳酸中毒,行政院衛生署雖已於民國 67 年即禁用,然卻於某大陸藥品中檢出,因而引起我們研究的興趣。本研究係以氣相層析質譜儀定該成分,續以高效液相層析儀分析其含量。氣相層析質譜儀設定條件如下:HP-5MS 毛細氣相層析管, 以 70eV 離子電能作電子撞擊式 (EI mode) 分析, 起始溫度100 ℃維持 3 分鐘,再以每分鐘 10 ℃之升溫速率,至 280 ℃並維持 15 分鐘。高效液相層析分析條件如下:Cosmosil 5C18 AR (5 cm × 4.6 mm) 及μ Bondpak phenyl (30cm ×3.9 mm) 為分析之管柱, 使用移動相為磷酸二氫鉀 (pH 6.55): 乙?? (40:60)。 流速 1mL/min,偵測波長 235 nm。以 metformin 為內部標準品。分析結果如下:同日間及異日間之測試,其相對標準偏差在 1.6 %以下。偵測極限及最低檢出量分別為 0.065 μ g/mL 及0.20 μ g/mL,添加回收率 102.7 %,檢體中平均含量為 3.45mg ╱膠囊。
Phenformin was prohibited by the ROC Department of Health in 1978. Inthis investigation, a GC-MS was used for the detection of phenformin in herbalpreparation produced in Mainland China followed by determination by HPLC. ForGC-MS, a HP-5MS capillary column was used. The initial column temperature was at100 ℃ for 2 min, ramping 10 ℃ /min to 280 ℃, then holding at 280 ℃ for 15min. Ionization source temperature was at 230 ℃, and 70 eV electron impact modewas employed. HPLC was performed on a Cosmsil 5C18 AR (5 cm × 4.6 mm), and a μBondpak phenyl (30 cm × 3.9 mm)column using 0.01M potassium dihydrogenphosphate(pH 6.55)-ace- tonitrile (60:40, v/v) as eluent, with flow rate at 1.0 mL/minand detection wavelength set at 235 nm. Metformin was used as the internalstandard. The interday and intraday precisions were less than 1.6%. The limit ofdetection and the limit of quantitation were 0.065 μ g/mL and 0.20 μ g/mL,respectively, The spike recovery was 102.7%. The average content of phenforminin the preparation was 3.45 mag per capsule.