Supercritical fluid chromatographic separation method and device

A supercritical fluid and chromatographic separation technology, which is applied in the field of supercritical fluid chromatographic separation methods and devices, can solve problems such as difficult elution, band broadening, and decrease in resolution, and achieve the effects of convenient operation, elimination of interference, and improvement of contact

Pending Publication Date: 2022-02-08
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the samples are dissolved in the modifier, whose strength and viscosity do not match the SFC mobile phase, which often leads to band broadening, lower resolution and poor repeatability
This problem is more prominent in the preparation of SFC, and even the sample will have a process of precipitation and re-dissolution after injection, resulting in serious distortion of chromatographic peaks
In addition, when separating complex samples, the interference of impurities often becomes an obstacle to the efficient separation of SFC
The polarity distribution range of complex samples is wide, which increases the difficulty of sample dissolution, and some impurities are not easy to elute on SFC, which also causes troubles for separation

Method used

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  • Supercritical fluid chromatographic separation method and device
  • Supercritical fluid chromatographic separation method and device
  • Supercritical fluid chromatographic separation method and device

Examples

Experimental program
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Effect test

Embodiment 1

[0055] The materials and material specifications used in this embodiment are as follows:

[0056] Sample: the precipitate of Hedyotis diffusa after extraction with 95% ethanol and water sinking;

[0057] Chromatography packing: C18 (40μm, 100A);

[0058] Pre-separation device specification: 5mL;

[0059] Supercritical fluid preparative chromatographic column specification: 250×10mm i.d., 10μm.

[0060] The supercritical fluid chromatographic separation method of the present embodiment comprises the steps:

[0061] S1: Preparation of sample and chromatographic packing mixture

[0062] Weigh the dried powder of Hedyotis diffusa (100 g), add 95% ethanol (800 mL) with 8 times the ratio of solid to liquid, and extract twice under reflux, each time for 1 hour. The two extracts were combined and concentrated to 20 mL under reduced pressure with a rotary evaporator to obtain a dark green extract. Slowly add 100 mL of water to the extract under stirring condition, and after standi...

Embodiment 2

[0068] The materials and material specifications used in this embodiment are as follows:

[0069] Sample: the precipitate of Hedyotis diffusa after extraction with 95% ethanol and water sinking;

[0070] Chromatography packing: C18 (40μm, 100A);

[0071] Pre-separation device specification: 5mL;

[0072] Supercritical fluid preparative chromatographic column specification: 250×20mm i.d., 10μm.

[0073] The supercritical fluid chromatographic separation method of the present embodiment comprises the steps:

[0074] S1: Preparation of sample and chromatographic packing mixture

[0075] The preparation method of the Hedyotis diffusa sample is the same as in Example 1.

[0076] Weigh 1.0 g sample of Hedyotis diffusa into a mortar, add a small amount of ethanol to dissolve the sample. Subsequently, 3.0 g of C18 (40 μm, 100A) chromatographic filler was added to the solution, and after grinding evenly, the solvent was evaporated to prepare a mixture of the sample and the chromat...

Embodiment 3

[0082] The materials and material specifications used in this embodiment are as follows:

[0083] Sample: the precipitate of Hedyotis diffusa after extraction with 95% ethanol and water sinking;

[0084] Chromatographic packing: C8 (40μm, 100A);

[0085] Pre-separation device specification: 25mL;

[0086] Supercritical fluid preparative chromatographic column specification: 250×30mm i.d., 10μm.

[0087] The supercritical fluid chromatographic separation method of the present embodiment comprises the steps:

[0088] S1: Preparation of sample and chromatographic packing mixture

[0089] The preparation method of the Hedyotis diffusa sample is the same as in Example 1.

[0090]Weigh 2.0 g of Hedyotis diffusa sample into a mortar, add a small amount of ethanol to dissolve the sample. Subsequently, 8.0 g of C8 (40 μm, 100A) chromatographic filler was added to the solution, and after grinding evenly, the solvent was evaporated to prepare a mixture of the sample and the chromato...

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Abstract

The invention discloses a supercritical fluid chromatographic separation method and device. The supercritical fluid chromatographic separation method comprises the following steps: placing a sample in a pre-separation device; connecting one end of a pre-separation device with a chromatographic column front pipeline, and connecting the other end of the pre-separation device with a supercritical fluid preparation chromatographic column; pre-separating a sample by taking supercritical carbon dioxide as an extraction solvent, and loading a pre-separated target component to a supercritical fluid preparation chromatographic column; connecting the chromatographic column front pipeline to the supercritical fluid preparation chromatographic column; taking supercritical carbon dioxide and a modifier as mobile phases, and separating target components. According to the supercritical fluid chromatography separation method, extraction, pretreatment, sample loading and separation of the sample can be completed in one step, the problem that the strength and viscosity of a sample dissolving reagent in supercritical fluid chromatography are not matched with those of a mobile phase is solved, and interference of a sample loading solvent and impurities in the sample on supercritical fluid chromatography separation is eliminated.

Description

technical field [0001] The application relates to the technical field of chromatography, in particular to a supercritical fluid chromatography separation method and device. Background technique [0002] In recent years, environmentally friendly subcritical / supercritical carbon dioxide (Sc-CO 2 ) as the mobile phase of supercritical fluid chromatography (Supercritical Fluid Chromatography, SFC) is considered to be a green, efficient and rapid separation technology. Compared with liquid chromatography (Liquid Chromatography, LC), SFC has a faster flow rate (about 3 times that of LC), higher separation throughput and lower organic solvent consumption. In particular, preparative SFC has certain advantages in sample purification due to its mild separation conditions, fast separation, and easy post-treatment. [0003] However, the dissolution of samples has always been a difficult problem in SFC separation. The mobile phase of SFC is composed of supercritical CO 2 And a certai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 金郁戴莹萍傅青柯燕雄
Owner EAST CHINA UNIV OF SCI & TECH
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