Method for preparing optically pure L-goitrin and D-goitrin by adopting liquid chromatogram and chiral separation analytical method
A technique for liquid chromatography and expressing Yichun, which is applied in the fields of preparing optically pure Glycin and expressing Yichun and chiral separation and analysis by liquid chromatography.
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Embodiment 1
[0041] Preparation of Optically Pure L-goitrin and D-goitrin Using SHISEIDO CD-PH Analytical Column
[0042] 1. Instruments and Materials
[0043] Reagents: n-hexane, ethanol (Shanghai Zhenxing Factory, analytical grade); DL-goitrin standard sample (Acros Organics Company, >99%).
[0044] Instruments: Waters 600 pump, waters 486 dual-wavelength ultraviolet detector, Junrui chromatographic workstation; CD-PH column (SHISEIDO, 250*4.6mm); rotary evaporator (Shanghai Yuhua Instrument Co., Ltd.); circulating water pump (Shanghai Yuhua Instrument Co., Ltd.); Kang Kejiao Instrument Equipment Co., Ltd.); Jasco P-1000 series digital automatic polarimeter (JASCO Japan).
[0045] 2. Preparation method
[0046] Dissolve 30mg of DL-goitrin standard sample in 15ml of ethanol. Separation with analytical SHISEIDO CD-PH column (250*4.6mm), high performance liquid chromatography conditions: mobile phase adopts n-hexane-ethanol system (70 / 30, v / v), flow rate is 1.0ml / min, detection wavelengt...
Embodiment 2
[0049] Preparation of optically pure L-goitrin and D-goitrin with SHISEIDO CD-PH semi-preparative column
[0050] 1. Instruments and Materials
[0051] Reagents: n-hexane, ethanol (Shanghai Zhenxing Factory, analytical grade); DL-goitrin standard sample (Acros Organics Company, >99%).
[0052] Instruments: Waters 600 pump, waters 486 dual-wavelength ultraviolet detector, Junrui chromatographic workstation; CD-PH column (SHISEIDO, 250*9.4mm); rotary evaporator (Shanghai Yuhua Instrument Co., Ltd.); circulating water pump (Shanghai Yuhua Instrument Co., Ltd.); Kang Kejiao Instrument Equipment Co., Ltd.).
[0053] 2. Preparation method
[0054] Dissolve 120mg of DL-goitrin standard sample in 60ml of ethanol. Separation with preparative SHISEIDO CD-PH semi-preparative column (250*9.4mm), liquid chromatography conditions: mobile phase adopts n-hexane-ethanol system (70 / 30, v / v), flow rate is 4.0ml / min, detection The wavelength is 244nm. Inject 1ml each time, and collect fracti...
example 3
[0056] Preparation of Optically Pure L-goitrin and D-goitrin Using DAICEL CHIRALPAK AD-RH Analytical Column
[0057] 1. Instruments and Materials
[0058] Reagents: Methanol (Merck, chromatographically pure); the mobile phase and the water used for preparing the solution are Watsons distilled water; DL-goitrin standard sample (Acros Organics Company, >99%).
[0059] Instruments: Waters 600 pump, waters 486 dual-wavelength ultraviolet detector; Millenium 32 workstation; CHIRALPAK AD-RH column (Daicel Chemistry Industry, 150*4.6mm); rotary evaporator (Shanghai Yuhua Instrument Co., Ltd.); circulating water pump ( Shanghai Yukang Science and Education Equipment Co., Ltd.).
[0060] 2. Preparation method
[0061] Dissolve 30mg of DL-goitrin standard sample in 4ml of distilled water. With CHIRALPAKAD-RH column (Daicel Chemistry Industry, 150*4.6mm), high-performance liquid chromatography conditions are: mobile phase adopts methanol-water system (30 / 70, v / v), flow rate is 1.0ml / m...
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