CAJ | 학술논문

运用高速逆流色谱( HSCCC)技术从太白贝母中分离制备贝母辛。以正己烷/乙酸乙酯/甲醇/水(体积比4∶5∶3∶5)为溶剂体系,转速800 r/min,流速2.0 mL/min,温度35℃,检测波长为215 nm,从50 mg太白贝母总生物碱中经一次HSCCC分离可得到5.3 mg贝母辛,纯度为96.3%,回收率为87.2%。并利用高效液相色谱-四极杆飞行时间质谱(HPLC-QTOF MS)对贝母辛进行了结构确证。
운용고속역류색보( HSCCC)기술종태백패모중분리제비패모신。이정기완/을산을지/갑순/수(체적비4∶5∶3∶5)위용제체계,전속800 r/min,류속2.0 mL/min,온도35℃,검측파장위215 nm,종50 mg태백패모총생물감중경일차HSCCC분리가득도5.3 mg패모신,순도위96.3%,회수솔위87.2%。병이용고효액상색보-사겁간비행시간질보(HPLC-QTOF MS)대패모신진행료결구학증。
Peimisine, an isosteroidal alkaloid occurring in Fritillaria species, is a semi-synthetic precursor of cyclopamine. In this paper, high-speed counter-current chromatography ( HSCCC) was applied to the separation and purification of peimisine from Fritillaria taipaiensis bulbs. The separation was performed on a TBE-300B HSCCC machine, by using solvent system of n-hexane-ethyl and acetate-methanol-water (4∶5∶3∶5, volume ratio) at 35 ℃, rotating speed 800 r/min, flow rate 2. 0 mL/min, and detection wavelength 215 nm. After a HSCCC run, 5. 3 mg of target compound was obtained from 50 mg of total alkaloid extract, with the purity of 96. 3% and the recovery of 87. 2%. The structure of the isolate was confirmed by high performance liquid chromatography-quadruple time-of-flight tandem mass spectrometry ( HPLC-QTOF MS) .