Multi-center cutting separation method for traditional Chinese medicines

A separation method and multi-center technology, applied in material separation, analysis materials, measurement devices, etc., can solve the problems of low sensitivity and resolution of trace compound analysis, achieve increased extraction efficiency, convenient repeatability, and simple operation steps clear effect

Active Publication Date: 2020-07-14
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the problem of low analytical sensitivity and resolution of trace compounds in traditional Dendrobium plants, the present invention provides a high-sensitivity multi-heart-cutting separation method for traditional Chinese medicine

Method used

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  • Multi-center cutting separation method for traditional Chinese medicines
  • Multi-center cutting separation method for traditional Chinese medicines
  • Multi-center cutting separation method for traditional Chinese medicines

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Refer to figure 1 The process flow chart of the above is that the dendrobium candidum is pulverized and passed through a No. 3 sieve to obtain the dendrobium candidum powder;

[0041] (2) Take a clean agate mortar, add 25 mg of Dendrobium officinale powder, then accurately weigh 25 mg of the dispersant, add it into the mortar respectively, and grind for 5 minutes to obtain a mixture;

[0042] (3) The fully ground mixture is transferred to the solid-phase extraction column of polypropylene;

[0043] (4) Elute the Dendrobium officinale powder and dispersant mixture with 200 μL methanol at a flow rate of 0.3 mL / min, and elute it into a 1.5 mL centrifuge tube;

[0044] (5) Place the 1.5mL centrifuge tube in an ultra-high-speed centrifuge, centrifuge at 12000rpm for 10 minutes, take the supernatant and load it for sample analysis. According to the above conditions, two Agilent 1290 ultra-high performance liquid 6545 mass spectrometry was used to determine the active in...

Embodiment 2

[0046] (1) Refer to figure 1 The process flow chart of the above is that the dendrobium candidum is pulverized and passed through a No. 3 sieve to obtain the dendrobium candidum powder;

[0047] (2) Take a clean agate mortar, add 25 mg of Dendrobium officinale powder, then accurately weigh 25 mg of the dispersant, add it into the mortar respectively, and grind for 5 minutes to obtain a mixture;

[0048] (3) The fully ground mixture is transferred to the solid-phase extraction column of polypropylene;

[0049] (4) Elute the Dendrobium officinale powder and dispersant mixture with 200 μL methanol at a flow rate of 0.5 mL / min, and elute it into a 1.5 mL centrifuge tube;

[0050] (5) Place the 1.5mL centrifuge tube in an ultra-high-speed centrifuge, centrifuge at 13000rpm for 8 minutes, take the supernatant and load it for sample analysis. According to the above conditions, two Agilent 1290 ultra-high performance liquid 6545 mass spectrometry was used to determine the active ing...

Embodiment 3

[0052] (1) Refer to figure 1 The process flow chart of the above, the Dendrobium nobile is pulverized, and the No. 3 sieve is passed to obtain the Dendrobium nobile powder;

[0053] (2) Take a clean agate mortar, add 25 mg of Dendrobium nobile powder, then accurately weigh 50 mg of the dispersant, add it into the mortar, grind for 10 minutes, and obtain the mixture;

[0054] (3) The fully ground mixture is transferred to the solid-phase extraction column of polypropylene;

[0055] (4) Elute the Dendrobium nobile powder and dispersant mixture with 200 μL methanol at a flow rate of 0.4 mL / min, and elute into a 1.5 mL centrifuge tube;

[0056] (5) Place the 1.5mL centrifuge tube in an ultra-high-speed centrifuge, centrifuge at 13500rpm for 5 minutes, take the supernatant liquid and load it for sample analysis. According to the above conditions, two Agilent 1290 ultra-high performance liquid 6545 mass spectrometry was used to determine the active ingredients in traditional Chine...

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Abstract

The invention relates to the technical field of traditional Chinese medicine effective component separation, and provides a multi-center cutting separation method for traditional Chinese medicines inorder to solve the problems of low analysis sensitivity and low resolution of trace compounds in traditional dendrobium plants, and the method comprises the following steps: (1) crushing raw materialtraditional Chinese medicinal materials, and sieving with a No.3 sieve to obtain traditional Chinese medicine powder; (2) mixing and grinding the traditional Chinese medicine powder and a dispersing agent to obtain a mixture; and (3) filling the mixture into a small solid-phase extraction column, and analyzing the separation effect through elution, centrifugation and sample introduction. Accordingto the method, under a multi-center cutting mode, effective components in dendrobium officinale, dendrobium stem and dendrobium chrysotoxum are separated and identified by utilizing 2D-LC-QTOF-MS andare ingeniously combined, and trace components in traditional Chinese medicines can be conveniently and efficiently separated.

Description

technical field [0001] The invention relates to the technical field of separation of effective components of traditional Chinese medicine, in particular to a multi-heart-cutting separation method of traditional Chinese medicine. Background technique [0002] Two-dimensional ultra-high performance liquid chromatography is an ideal and powerful analytical tool that has attracted enormous interest. In the two-dimensional ultra-high performance liquid chromatography system, the multiple heart-cutting mode occupies the main position. In the multiple heart-cutting mode, only a specific portion of the sample separated from the 1D column is transferred to the 2D column for secondary separation and detection. In general, the total run time in 2D is longer than the collection time in 1D in multiple heart-cut mode. At the same time, on this basis, two-dimensional ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (Q-TOF-MS) aims to g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 曹君王秋燕胡雨涵杨娟
Owner HANGZHOU NORMAL UNIVERSITY
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