Method for preparing flavanone glycoside compound by using industrial chromatographic technology

Abstract

The invention discloses a method for preparing a flavanone glycoside compound by using an industrial chromatographic technology, which comprises the following steps: taking a sample solution of a total flavonoid glycoside extract as a raw material, purifying by using an industrial chromatographic technology dynamic axial compression column system, and detecting the separation condition by using a dual-wavelength ultraviolet online detector, and according to the appearance time and the chromatographic peak height of the shaddock peel rutin component, collecting the eluent of the prepared flavanone glycoside compound with the collection starting and ending time of 155-235 min, and concentrating and drying the eluent. The purity of the prepared flavanone glycoside compound is relatively high; and the method has the characteristics of good process reproducibility, simplicity in operation, short preparation time, less organic solvent dosage, economy, environmental protection, large-scale industrial production and the like.

Description

technical field

[0001] The invention belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines, and in particular relates to a method for preparing dihydroflavone glycosides by using industrial chromatographic technology. Background technique

[0002] Naringe rutin is a kind of dihydroflavonoid glycosides. According to literature reports, it is widely found in traditional Chinese medicinal materials such as Fructus Aurantii Fructus, Citrus Aurantium, Changshan Huyou, Huazhou Pomelo, Huajuhong, etc. Huaqi Tablets, Chenxianglu Bailu Tablets, Xiaoer Fupi Granules, Weisu Granules, Zhishi Xiaopi Pills, Huoxiang Zhengqi Oral Liquid and other dozens of Chinese medicine varieties are used as active ingredients or representative ingredients for quality control. However, the research on low-content components such as naringel rutin is not enough, and due to the low content of this component and the cumbersome and complicated s...

Examples

Embodiment 1

[0027] A kind of method that utilizes industrial chromatographic technology to prepare dihydroflavonoid glycoside compound naringin rutin, process flow chart is as follows figure 1 As shown, the specific steps are as follows:

[0028] Get the total flavonoid glycosides extract of Fructus Aurantii (its HPLC chromatogram sees figure 2 ), wherein the naringin rutin content is about 3.5% (W / W), add 4.0% (V / V) acetonitrile aqueous solution to dissolve it and be formulated with a solution of 125mg / ml, filter, and set aside to obtain a sample solution; the sample Solution 90L, injected into the dynamic axial compression column system, the industrial chromatographic filler is UniPSN 40-300 (reverse polymer filler), acetonitrile:water:phosphoric acid solution (15:85:0.1, V / V / V) is the elution reagent, the elution flow rate is 2000mL / min, the ultraviolet detection wavelength is 283nm, and the reference wavelength is 210nm. According to the peak time of naringel rutin components and t...

Embodiment 2

[0030] A kind of method that utilizes industrial chromatographic technology to prepare dihydroflavonoid glycoside compound naringin rutin, process flow chart is as follows figure 1 As shown, the specific steps are as follows:

[0031] Get the total flavonoid glycoside extract of Fructus Aurantii, wherein the naringin rutin content is about 2.5% (W / W), add 3.0% (V / V) acetonitrile aqueous solution to dissolve it and prepare a solution of 85 mg / ml, filter to obtain Sample solution: inject 115L of sample solution into the dynamic axial compression column system, the industrial chromatographic filler is UniPS 40-300 (reverse polymer filler), acetonitrile: water: phosphoric acid solution (25:75:0.1, V / V / V) is the eluent, the elution flow rate is 1500mL / min, the ultraviolet detection wavelength is 283nm, and the reference wavelength is 210nm. According to the peak time of naringel rutin components and the height of the chromatographic peak, the eluent of the prepared naringelin rut...

Embodiment 3

[0033] A kind of method that utilizes industrial chromatographic technology to prepare dihydroflavonoid glycoside compound naringin rutin, process flow chart is as follows figure 1 As shown, the specific steps are as follows:

[0034] Get the total flavonoid glycoside extract of Fructus Aurantii, wherein the naringin rutin content is about 2.0% (W / W), add water to dissolve it and prepare a 100mg / ml solution, filter to obtain a sample solution; sample solution 100L, Inject into the dynamic axial compression column system, the industrial chromatographic filler is or CG161M (reversed-phase polymer filler), acetonitrile:water:phosphoric acid solution (18:82:0.1, V / V / V) is the eluent, and the elution flow rate is It is 1750mL / min, the ultraviolet detection wavelength is 283nn, and the reference wavelength is 210nm. According to the peak time of naringel rutin components and the height of the chromatographic peak, the eluent of the prepared naringelin rutin was collected, and the c...

technical field

[0001] The invention belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines, and in particular relates to a method for preparing dihydroflavone glycosides by using industrial chromatographic technology. Background technique

[0002] Naringe rutin is a kind of dihydroflavonoid glycosides. According to literature reports, it is widely found in traditional Chinese medicinal materials such as Fructus Aurantii Fructus, Citrus Aurantium, Changshan Huyou, Huazhou Pomelo, Huajuhong, etc. Huaqi Tablets, Chenxianglu Bailu Tablets, Xiaoer Fupi Granules, Weisu Granules, Zhishi Xiaopi Pills, Huoxiang Zhengqi Oral Liquid and other dozens of Chinese medicine varieties are used as active ingredients or representative ingredients for quality control. However, the research on low-content components such as naringel rutin is not enough, and due to the low content of this component and the cumbersome and complicated s...

Examples

Embodiment 1

[0027] A kind of method that utilizes industrial chromatographic technology to prepare dihydroflavonoid glycoside compound naringin rutin, process flow chart is as follows figure 1 As shown, the specific steps are as follows:

[0028] Get the total flavonoid glycosides extract of Fructus Aurantii (its HPLC chromatogram sees figure 2 ), wherein the naringin rutin content is about 3.5% (W / W), add 4.0% (V / V) acetonitrile aqueous solution to dissolve it and be formulated with a solution of 125mg / ml, filter, and set aside to obtain a sample solution; the sample Solution 90L, injected into the dynamic axial compression column system, the industrial chromatographic filler is UniPSN 40-300 (reverse polymer filler), acetonitrile:water:phosphoric acid solution (15:85:0.1, V / V / V) is the elution reagent, the elution flow rate is 2000mL / min, the ultraviolet detection wavelength is 283nm, and the reference wavelength is 210nm. According to the peak time of naringel rutin components and t...

Embodiment 2

[0030] A kind of method that utilizes industrial chromatographic technology to prepare dihydroflavonoid glycoside compound naringin rutin, process flow chart is as follows figure 1 As shown, the specific steps are as follows:

[0031] Get the total flavonoid glycoside extract of Fructus Aurantii, wherein the naringin rutin content is about 2.5% (W / W), add 3.0% (V / V) acetonitrile aqueous solution to dissolve it and prepare a solution of 85 mg / ml, filter to obtain Sample solution: inject 115L of sample solution into the dynamic axial compression column system, the industrial chromatographic filler is UniPS 40-300 (reverse polymer filler), acetonitrile: water: phosphoric acid solution (25:75:0.1, V / V / V) is the eluent, the elution flow rate is 1500mL / min, the ultraviolet detection wavelength is 283nm, and the reference wavelength is 210nm. According to the peak time of naringel rutin components and the height of the chromatographic peak, the eluent of the prepared naringelin rut...

Embodiment 3

[0033] A kind of method that utilizes industrial chromatographic technology to prepare dihydroflavonoid glycoside compound naringin rutin, process flow chart is as follows figure 1 As shown, the specific steps are as follows:

[0034] Get the total flavonoid glycoside extract of Fructus Aurantii, wherein the naringin rutin content is about 2.0% (W / W), add water to dissolve it and prepare a 100mg / ml solution, filter to obtain a sample solution; sample solution 100L, Inject into the dynamic axial compression column system, the industrial chromatographic filler is or CG161M (reversed-phase polymer filler), acetonitrile:water:phosphoric acid solution (18:82:0.1, V / V / V) is the eluent, and the elution flow rate is It is 1750mL / min, the ultraviolet detection wavelength is 283nn, and the reference wavelength is 210nm. According to the peak time of naringel rutin components and the height of the chromatographic peak, the eluent of the prepared naringelin rutin was collected, and the c...

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