高速逆流色谱分离制备白胡椒中单萜类化合物

Study on the Separation of Monoterpenes from Piper nigrum L. by High-speed Counter-current Chromatography

应用高速逆流色谱法分离制备了白胡椒中3种单萜类化合物。以V(叔丁基甲基醚)∶V(甲醇)∶V(水)=2∶1∶1为两相溶剂系统,上相为固定相,下相为流动相,在主机转速900 r/min、流动相流速2.5 mL/min条件下,从2.76 g样品中一步分离制备得到3,7-二甲基-2-辛烯-1,6,7-三醇35 mg,对薄荷烷-1,2,8-三醇-2-O-β-D葡萄糖苷55mg,5-羟基龙脑-2-O-β-D葡萄糖苷40mg,经高效液相蒸发光散射检测器(HPLC-ELSD)检测纯度均达95.0%以上,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。研究结果表明,利用该方法可以对白胡椒中的单萜类化合物进行快速的分离和纯化,且制备量大,分离效率高。

Three monoterpenes were prepared, isolated and purified from Piper nigrum L.. by high-speed counter-current ehromatography（HSCCC） . A two-phase solvent system composed of TBME-methanol-water （2： 1： 1, v/v/ v） was used. The upper phase was stationary phase and lower phase was mobile phase. By one-step elution, under the conditions of a flow rate of 2.5 mL/min and 900 r/rain, 35 mg of 3,7-dimethyloct-2E-en-1,6,7-triol, 55 mg of p-menthane-1,2,8-triol-2-O-β-D-glueopyranoside and 40 mg of 5-hydroxy bornyl-2-O-β-D-glucopyranoside was obtained from 2.76 mg of the butanol extract of Piper nigrum L. ,the purities was over 95.0% detected by high performance liquid chromatography with evaporative light scattering detection. The obtained fractions were analyzed by high performance liquid chromatography （HPLC） , and identified by mass spectrometry （MS） , 1H-nuclear magnetic resonance （NMR） and Z3C-NMR. The results indicated that HSCCC is a powerful technique for the purification of monoterpenes from Piper nigrum L. with high productive capacity and high efficiency.