蛇床子藥材中蛇床子素之分離暨氣相層析定量   全文下載

Isolation and Gas Chromatographic Method for Determination of Osthole from Cnidii Fructus

本研究的目的是探討蛇床子藥材中蛇床子素（osthole）之分離與定量，建立氣相層析法檢測多種不同來源蛇床子藥材中蛇床子素之含量。分別以6種溶媒抽提蛇床子藥材，評估抽提效率，並比較真空減壓分段蒸餾法與傳統管柱法純化取得蛇床子素之效益。所建立之氣相層析法係以氮氣為移動相，流速為40 mL／min，分流比120：1，以DB?-5為分析管柱（30 m × 0.53 mm L.D.，1.5μm），FID檢測器，升溫程式為起始溫度135℃維持12 min，升溫段：12℃／min，末段溫度215℃維持20 min，蛇床子素之滯留時間為24.1 min，內部標準品為無水咖啡因（caffeine anhydrous），滯留時間為18.9 min。結果顯示以乙醇抽提蛇床子素之效率最佳，水的抽提效果最差。真空減壓分段蒸餾法較適合用於純化取得蛇床子素。台灣市售蛇床子之蛇床子素含量為2.14%至0.05%；而中國大陸南方蛇床子之蛇床子素含量較北方所產者為高。

The purpose of this research is to study the isolation and purification of osthole from Cnidii Fructus extract and to establish a gas chromatographic method for determining the osthole content from various Cnidii Fructus samples. Six solvents were used to extract Cnidii Fructus in order to evaluate their efficiency in extracting osthole. Vacuum fractional distillation and traditional column chromatography were compared to evaluate the efficiency in purifying osthole from Cnidii Fructus extract. Gas chromatographic method was used to determine osthole content in Cnidii Fructus extract. The analytical conditions are the following: nitrogen as the carrier gas, the flow rate of 40 mL/min; the split ratio of 120 : 1. The column used was DBTM-5 (30 m × 0.53 mm I.D., 1.5 μm) equipped with a flame ionization detector (FID). The initial oven temperature was programmed to be at 135°C for 12 minutes. The temperature was then raised to 215°C at a rate of 12°C /min for 20 minutes. The retention time of osthole was 24.1 min. Caffeine anhydrous was used as the internal standard with a retention time of 18.9 minutes. A comparative evaluation showed that aqueous alcoholic solvent was the most efficient solvent among six used in extraction of osthole from a Cnidii Fructus. Vacuum fractional distillation is useful for purifying osthole from Cnidii Fructus extract. It was found that the osthole content of commercial Cnidii Fructus samples varied from 0.05% to 2.14%. And the osthole content of Cnidii Fructus samples collected from Southern China was higher than those collected from Northern China. 本研究的目的是探討蛇床子藥材中蛇床子素（osthole）之分離與定量，建立氣相層析法檢測多種不同來源蛇床子藥材中蛇床子素之含量。分別以6種溶媒抽提蛇床子藥材，評估抽提效率，並比較真空減壓分段蒸餾法與傳統管柱法純化取得蛇床子素之效益。所建立之氣相層析法係以氮氣為移動相，流速為40 mL／min，分流比120：1，以DB™-5為分析管柱（30 m × 0.53 mm L.D.，1.5μm），FID檢測器，升溫程式為起始溫度135℃維持12 min，升溫段：12℃／min，末段溫度215℃維持20 min，蛇床子素之滯留時間為24.1 min，內部標準品為無水咖啡因（caffeine anhydrous），滯留時間為18.9 min。結果顯示以乙醇抽提蛇床子素之效率最佳，水的抽提效果最差。真空減壓分段蒸餾法較適合用於純化取得蛇床子素。台灣市售蛇床子之蛇床子素含量為2.14%至0.05%；而中國大陸南方蛇床子之蛇床子素含量較北方所產者為高。