目的 分析黃柏在不同溫度下進(jìn)行模擬炮制后, 不同炮制品中主要化學(xué)成分的變化情況, 為解析黃柏不同炮制品的科學(xué)內(nèi)涵提供參考依據(jù)。方法 采用高效液相色譜法檢測黃柏不同炮制品中生物堿類成分小檗堿、小檗紅堿、黃柏堿、藥根堿、巴馬汀和檸檬苦素類成分黃柏內(nèi)酯、黃柏酮。生物堿類成分檢測的色譜條件為Ecosil C₁₈色譜柱(250 mm×4.6 mm, 5 μm);流動(dòng)相:乙腈-0.1%磷酸水(50:50)(每100 mL 0.1%磷酸水加十二烷基硫酸鈉0.4 g);檢測波長:284 nm;體積流量:1 mL/min;柱溫:35 ℃;進(jìn)樣量:3 μL。檸檬苦素類成分檢測的色譜條件為Ecosil C₁₈色譜柱(250 mm×4.6 mm, 5 μm);流動(dòng)相:乙腈-水-磷酸(45:55:0.2);檢測波長:210 nm;體積流量:1 mL/min;柱溫:35 ℃;進(jìn)樣量:10 μL。結(jié)果 直接烘制品、水潤烘制品、酒潤烘制品、鹽水潤烘制品在最佳炮制溫度160 ℃下, 總生物堿的質(zhì)量分?jǐn)?shù)分別為3.009 6%、2.993 1%、3.989 6%、4.537 9%, 其中酒潤烘制品和鹽水潤烘制品均較生品3.528 2%高, 提示黃柏經(jīng)輔料炮制后有利于生物堿類成分的溶出, 且增加溶出率的是輔料鹽和酒, 而非水。當(dāng)炮制溫度達(dá)到160 ℃以上時(shí), 在相應(yīng)炮制溫度下的直接烘制品和水潤烘制品中檸檬苦素類成分質(zhì)量分?jǐn)?shù)未見明顯差異, 酒潤烘制品和鹽水潤烘制品隨著溫度的升高其質(zhì)量分?jǐn)?shù)相差較大, 提示水對(duì)黃柏炮制過程中的檸檬苦素類成分基本沒有影響, 酒、鹽炮制具有影響。結(jié)論 黃柏經(jīng)炮制后生物堿類和檸檬苦素類成分會(huì)發(fā)生量變和質(zhì)變, 輔料和溫度對(duì)其成分的變化有直接的影響, 本研究可為黃柏炮制后藥性發(fā)生改變與其化學(xué)成分的變化具有相關(guān)性提供參考和依據(jù)。

Objective To study the variation of the main components in Phellodendri Cortex processed with different methods and temperature, and to provide scientific references for processing principle. Methods The contents of alkaloids (berberine, berberrubine, phellodendrine, jatrorrhizine, and palmatine) and limonoids (obaculactone and obacunone) from different processed products were determined by HPLC method. Alkaloids determination were carried out on an Ecosil C₁₈ column (250 mm × 4.6 mm, 5 μm) with acetonitrile-0.1% phosphoric acid water (50:50) (added 0.4 g SDS to 0.1% phosphoric acid water per 100 mL) as mobile phase. The detection wavelength was 284 nm and injection volume was 3 μL at the flow rate of 1.0 mL/min. The column temperature was set for 35 ℃. An Ecosil C₁₈ column (250 mm × 4.6 mm, 5 μm) was used for determination of limonoids. Mobile phase was consisted of acetonitrile-water-phosphoric acid (45:55:0.2), and it was monitored at a wavelength of 210 nm. The column temperature was 35 ℃, and the injection volume was 10 μL at a flow rate of 1.0 mL/min. Results At the optimal temperature 160 ℃, the total alkaloids in Phellodendri Cortex direct drying product, processed products with water, rice-wine, and salt-water were 3.009 6%, 2.993 1%, 3.989 6%, and 4.537 9%, respectively. Contents of the total alkaloids in processed products with rice-wine and salt-water were above that of raw product with 3.528 2%. It was suggested that it was rice-wine and salt-water, not water which improved dissolution of total alkaloids in Phellodendri Cortex. When the temperature is above 160 ℃, the total contents of limonoids in processed products with water and direct drying products were similar, but the processed products with rice-wine and salt-water were large difference with the increase of temperature. It was also suggested that it was accessories rice-wine and salt-water, not water which improved dissolution of the total contents of limonoids in Phellodendri Cortex. Conclusion After procession, alkaloids and limonoids have qualitative and quantitative change, and the accessories and temperature have directly influence on the change of their contents. It would provide reference and basis to the correlation between the properties change and the chemical components variation from Phellodendri Cortex after processing.

國家自然科學(xué)基金資助項(xiàng)目(81274083)