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Method for simultaneously detecting five anthraquinone compounds in polygonum multiflorum based on combination of solid-phase dispersion extraction and ultra-high performance liquid chromatography

An ultra-high-efficiency liquid phase and solid phase dispersion technology, applied in the field of analysis, can solve problems such as chromatographic column damage, co-extraction measurement interference, and complex matrix of Chinese herbal medicines.

Pending Publication Date: 2021-07-06
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sample pretreatment process only has an extraction process, but no purification process. Although it is simple and fast, due to the complex matrix of Chinese herbal medicines, the interference caused by co-extraction to the determination and the damage to the chromatographic column cannot be ignored.

Method used

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  • Method for simultaneously detecting five anthraquinone compounds in polygonum multiflorum based on combination of solid-phase dispersion extraction and ultra-high performance liquid chromatography
  • Method for simultaneously detecting five anthraquinone compounds in polygonum multiflorum based on combination of solid-phase dispersion extraction and ultra-high performance liquid chromatography
  • Method for simultaneously detecting five anthraquinone compounds in polygonum multiflorum based on combination of solid-phase dispersion extraction and ultra-high performance liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0021] An Acquity UPLC H-Class Plus ultra-high performance liquid chromatograph (U.S. waters company) was used, equipped with an Acquity quaternary gradient pump, an Acquity FTN autosampler, an Acquity column oven and an Acquity FDA diode array detector. Chromatographic conditions: Chromatographic column: ACQUITY UPLC ® HSS T3 analytical column (2.1mm×100 mm×1.8 μm); column temperature: 35°C; injection volume: 5μL; mobile phase: phase A is water (containing 0.1% formic acid), Phase B is acetonitrile (containing 0.1% formic acid), the gradient elution program is shown in Table 1; flow rate: 0.4 mL / min; detection wavelength: 254 nm.

[0022] Table 1 Gradient elution program

[0023]

Embodiment 2

[0025] Prepare mixed standard solutions of 5 kinds of anthraquinone compounds with a series of mass concentrations, and measure them under the above-mentioned chromatographic conditions. Draw a standard curve with the peak area Y of each component against the mass concentration X (see Table 2), and the 5 target compounds are linearly good linearity over the range ng (R 2 >0.9964), the limit of detection (LOD) and limit of quantification (LOQ) were in the range of 0.01-0.07 mg / L and 0.04-0.28 mg / L, respectively.

[0026] Table 2 Linear equation, detection limit and quantification limit of 5 kinds of anthraquinone compounds

[0027]

Embodiment 3

[0029] Sample pretreatment: Weigh 0.5 g (accurate to 0.001 g) of Polygonum multiflorum, add 30 mL of 70% methanol, ultrasonically extract for 30 min, centrifuge at 5000 rpm for 5 min, take the supernatant, dilute with water to make the methanol content 50% . Take 5mL of the above extract, add 0.6 g C 18 Adsorb the material, vortex and oscillate for 10 min, centrifuge at 10,000 rpm for 10 min, collect the C18 material, and repeat the above adsorption steps twice with the C18 material in the supernatant. C used for merging 3 times 18 The material was ultrasonically eluted with 20 mL of acetonitrile for 30 min, centrifuged at 10,000 rpm for 10 min, the supernatant was taken out, dried with nitrogen, the residue was reconstituted with 0.5 mL of methanol, and passed through a 0.22 μm filter membrane for UPLC-DAD analysis.

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Abstract

The invention discloses an ultra-high performance liquid chromatography-diode array method (UPLC-DAD) for simultaneously detecting five anthraquinone compounds (emodin, physcion, chrysophanol, rhein and aloe-emodin) in polygonum multiflorum. The polygonum multiflorum is used as a traditional tonifying medicine and has a long history. The anthraquinone compound is a main natural medicine component in polygonum multiflorum, has the functions of antibiosis, anti-inflammation, immunoregulation and cardiovascular protection, and is mainly composed of emodin, physcion, chrysophanol, rhein and aloe-emodin. According to the method, a dispersive solid-phase extraction (DSPE) method is adopted, a UPLC-DAD analysis technology is combined, a novel analysis method for simultaneously detecting the five anthraquinone compounds in the polygonum multiflorum is provided, the detection limit of an instrument is 0.01-0.07 mg / L, and a technical means is provided for quality control and safety evaluation of the polygonum multiflorum medicinal material.

Description

technical field [0001] The invention relates to a simultaneous detection of five anthraquinone compounds (emodin, emodin methyl ether, chrysophanol, rhein and aloe rhubarb) in Polygonum multiflorum based on solid phase dispersion extraction (DSPE) combined with ultra-high performance liquid chromatography-diode array method element) analysis method, belongs to the field of analysis technology. Background technique [0002] Polygonum multiflorum is a traditional tonic medicine with activities such as hair growth and black hair, lipid regulation, anti-oxidation, anti-aging, anti-inflammation, anti-aging, neuroprotection, heart protection, liver protection, and immune regulation. It has long been used in the world It is widely used especially in Asian countries. Anthraquinone compounds are a kind of main natural medicinal ingredients in Polygonum multiflorum, mainly composed of emodin, emodin methyl ether, chrysophanol, rhein and aloe-emodin. [0003] With the increase of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/64G01N30/86
CPCG01N30/02G01N30/06G01N30/64G01N30/8679G01N2030/062
Inventor 万益群徐颖郭岚刘翻
Owner NANCHANG UNIV
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