CAJ | 학술논문

为满足天然产物高效分离的需求，本文研制了自动真空液相色谱（AUTO-VLC）装置并用于五味子石油醚萃取物的分离。该装置由自主设计的流动相储备系统、10通分流切换阀、3通切换阀、3个不同规格的动态轴向压缩色谱柱、10通馏分收集阀和馏分收集器组成，采用可编程逻辑控制器（PLC）S7-200实现了分离过程的不同比例流动相切换、不同规格色谱柱选择、分离时间设定及馏分收集的自动控制及监测。应用于五味子成分分离的结果表明：采用150mm直径动态轴向压缩色谱柱的VLC，从100g五味子石油醚萃取物中一次分离得到6个组成明显不同的样品（S1~S6）。建立了通过多次薄层色谱（TLC）展开筛选VLC分离条件的方法，并进行了分离验证。VLC分离条件选择方法：自动真空液相色谱的初始洗脱剂的比例以首次TLC展开时全部目标化合物的比移值（Rf）介于0~0. 45时展开剂的组成为宜；梯度洗脱比例变化以k值（展开次数（n）与Rf的线性函数斜率）和TLC分离度为依据选择；不同Rf范围内洗脱次数由n≈ΔRf／k计算。采用选择的条件从样品S5中分离得到了13个组分和4个纯度在85％以上的化合物，仅耗时17h。AUTO-VLC的研制对于中药成分的自动和系统性分离具有重要价值。
위만족천연산물고효분리적수구，본문연제료자동진공액상색보（AUTO-VLC）장치병용우오미자석유미췌취물적분리。해장치유자주설계적류동상저비계통、10통분류절환벌、3통절환벌、3개불동규격적동태축향압축색보주、10통류분수집벌화류분수집기조성，채용가편정라집공제기（PLC）S7-200실현료분리과정적불동비례류동상절환、불동규격색보주선택、분리시간설정급류분수집적자동공제급감측。응용우오미자성분분리적결과표명：채용150mm직경동태축향압축색보주적VLC，종100g오미자석유미췌취물중일차분리득도6개조성명현불동적양품（S1~S6）。건립료통과다차박층색보（TLC）전개사선VLC분리조건적방법，병진행료분리험증。VLC분리조건선택방법：자동진공액상색보적초시세탈제적비례이수차TLC전개시전부목표화합물적비이치（Rf）개우0~0. 45시전개제적조성위의；제도세탈비례변화이k치（전개차수（n）여Rf적선성함수사솔）화TLC분리도위의거선택；불동Rf범위내세탈차수유n≈ΔRf／k계산。채용선택적조건종양품S5중분리득도료13개조분화4개순도재85％이상적화합물，부모시17h。AUTO-VLC적연제대우중약성분적자동화계통성분리구유중요개치。
In order to meet the needs of efficient purification of products from natural resources,this paper developed an automatic vacuum liquid chromatographic device( AUTO-VLC)and applied it to the component separation of petroleum ether extracts of Schisandra chinensis(Turcz)Baill. The device was comprised of a solvent system,a 10-position distribu-tion valve,a 3-position changes valve,dynamic axis compress chromatographic columns with three diameters,and a 10-position fraction valve. The programmable logic controller( PLC)S7-200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection,separation time setting and fraction collection. The separation results showed that six fractions( S1-S6)of different chemical components from 100 g Schisandra chinensis ( Turcz)Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The ini-tial mobile phase of AUTO-VLC was selected by taking R f of all the target compounds ranging from 0 to 0.45 for fist development on the TLC;gradient elution ratio was selected according to k value(the slope of the linear function of Rf value and development times on the TLC)and the resolution of target compounds;elution times( n)were calculated by the formula n≈ΔR f/k. A total of four compounds with the purity more than 85% and 13 other components were separa-ted from S5 under the selected conditions for only 17 h. Therefore,the development of the au-tomatic VLC and its method are significant to the automatic and systematic separation of tradi-tional Chinese medicines.