CN-121994979-A - Plant sample centrifugation-free pretreatment method for magnetic particle-assisted solid-liquid rapid separation

Abstract

The invention discloses a centrifugal pretreatment-free method for plant samples with magnetic particle assisted solid-liquid rapid separation, which is characterized in that magnetic particles are added into a plant sample extraction system, the magnetic particles and insoluble solids are fully combined under the action of vortex mixing and/or ultrasonic treatment, then the solid-liquid rapid separation is realized under the action of an externally applied magnetic field, clear supernatant is obtained, and the traditional centrifugal operation is not needed to complete the pretreatment process of the samples. The method does not depend on high-speed centrifugal equipment, is simple and convenient to operate, has short treatment time, and is especially suitable for powdery or viscous plant samples. The sample extracting solution obtained by the invention can be directly used for gas chromatography-mass spectrometry or liquid chromatography-mass spectrometry analysis, and the analysis result has good consistency with the traditional centrifugation method. The invention can effectively reduce the dependence on centrifugal equipment, simplify the pretreatment flow of samples, improve the pretreatment efficiency of complex plant samples, and is suitable for the rapid detection and quality control of traditional Chinese medicine, spice, food and other plant source samples.

Inventors

• MAO DESHOU
• LEI SHENG
• CAI BINGBIAO
• ZHU LINGCHAO
• LI ZHIYU
• Zhu Cenming
• SONG CHUNMAN
• XIANG HAIYING
• XU LI
• LI XIANYI

Assignees

• 云南中烟工业有限责任公司

Dates

Publication Date

20260508

Application Date

20260224

Claims (9)

1. 1. The centrifugation-free pretreatment method for the plant sample with the assistance of magnetic particles for solid-liquid rapid separation is characterized by comprising the following steps: (1) Adding an extraction solvent into a plant sample to obtain a plant sample extraction system in which liquid and insoluble solids are mixed; (2) Adding magnetic particles into the plant sample extraction system, and enabling the magnetic particles to be contacted and combined with insoluble solids in the plant sample extraction system under the action of vortex mixing and/or ultrasonic treatment; (3) Under the action of an externally applied magnetic field, the magnetic particles and insoluble solids combined with the magnetic particles are aggregated and separated from a liquid phase to obtain clear supernatant; Wherein the method completes the solid-liquid separation of the plant sample extraction system without centrifugation.
2. 2. The method of claim 1, wherein the plant sample is a powdered, fibrous, granular or viscous plant source sample.
3. 3. The method according to claim 1 or 2, wherein the magnetic particles are magnetic metal oxide particles, magnetic composite particles; the particle size of the magnetic particles is nano-scale or micro-scale; The mass ratio of the plant sample to the magnetic particles is 1:5-1:15.
4. 4. A method according to claim 3, wherein the magnetic particles are Fe 3 O 4 magnetic particles; The magnetic particles are nano-sized, and the particle size of the magnetic particles is 20nm-100nm; when the plant sample is in a powder form, the mass ratio of the plant sample to the magnetic particles is 1:15, and when the plant sample is in a viscous form, the mass ratio of the plant sample to the magnetic particles is 1:5.
5. 5. The method according to claim 1, wherein the extraction solvent is methanol, ethanol, acetonitrile, dichloromethane, water or a mixed solvent of a plurality of the solvents in any ratio.
6. 6. The method of claim 1, wherein the time of the sonication is from 10 to 30min.
7. 7. The method of claim 1, wherein the externally applied magnetic field is provided by a permanent magnet or an electromagnet.
8. 8. The method of claim 1, wherein the supernatant is used directly in gas chromatography, liquid chromatography or analysis thereof in combination with mass spectrometry.
9. 9. The method according to claim 1, wherein the method is suitable for rapid detection and quality control of samples of herbal, spice, food plant origin.

Description

Plant sample centrifugation-free pretreatment method for magnetic particle-assisted solid-liquid rapid separation Technical Field The invention relates to the technical field of sample pretreatment and analysis detection, in particular to a centrifugation-free pretreatment method for plant samples with magnetic particle-assisted solid-liquid rapid separation, which is suitable for sample treatment of plant source samples before gas chromatography, liquid chromatography and combined mass spectrometry. Background The plant sample has wide application value in the fields of food, medicine, traditional Chinese medicine, spice, natural product analysis and the like, has complex chemical composition and usually contains volatile components, phenolic acids, flavonoids, alkaloids, polysaccharides, resins and other high molecular impurities. Prior to gas chromatography, liquid chromatography, and their combined mass spectrometry, plant samples are often subjected to a pretreatment to effect the efficient release of the target component, thereby obtaining a clear extract suitable for instrumental analysis. Currently, the most commonly used method in plant sample pretreatment is solvent extraction combined with centrifugation. Such methods typically involve adding an organic solvent to a plant source sample (e.g., a solid sample or a solid-liquid mixture), vortexing or ultrasonic extraction, followed by high-speed centrifugation to separate the solid sample residue from the organic solvent extract. However, the method has the problems of more operation steps, strong dependence on high-speed centrifugal equipment, complicated whole flow, long time consumption and the like. Especially when treating powdery, fibrous, granular or viscous plant samples, the centrifugation efficiency is easily affected by the physicochemical properties of the samples, and the conditions of unclear layering, turbid supernatant or repeated centrifugation are often occurred, so that the analysis efficiency is reduced and the repeatability and stability of the results are affected. In addition, the supernatant removal process after centrifugation has high requirements on the operation proficiency and is easily influenced by human factors. In the case of simultaneous processing of multiple batches of samples, the centrifugation step and manual removal of supernatant often become key bottlenecks limiting the throughput of the analysis, further increasing the experimental time costs and the labor costs. In recent years, magnetic materials have been introduced into the field of sample separation and enrichment because of their ability to achieve rapid response under the influence of an externally applied magnetic field. However, the related art of magnetic separation is mostly used for selective adsorption or magnetic solid phase extraction of target components, and generally, the subsequent magnetic separation operation is still required after the solvent extraction is completed and the supernatant is obtained by centrifugation. Aiming at the solid-liquid separation link in the pretreatment process of plant samples, particularly the centrifugal-free rapid separation of solid residues and extracting solution is realized, and general and simplified technical proposal report is not yet available. Therefore, there is still a need for a pretreatment method that has a simple structure, is convenient to operate, is suitable for multiple types of plant samples, and can achieve solid-liquid rapid separation and replace the conventional centrifugation step while guaranteeing the reliability of analysis results, thereby improving the efficiency and application range of pretreatment of plant samples. The present invention has been made to solve the above problems. Disclosure of Invention 1. Object of the invention Aiming at the problems that the prior plant sample pretreatment process generally depends on high-speed centrifugal equipment, has complicated operation steps, low treatment efficiency, unstable separation effect when treating powdery, fibrous, granular or sticky samples and the like, the invention aims to provide a plant sample centrifugation-free pretreatment method with magnetic particles for assisting in solid-liquid rapid separation. The method realizes the rapid separation of the solid residues and the extracting solution in the extracting process of the plant sample under the condition of not adopting centrifugal operation, thereby simplifying the pretreatment flow, reducing the equipment dependence and improving the pretreatment efficiency and the application range of the complex plant sample. 2. Technical proposal In order to achieve the aim of the invention, the invention adopts the following technical scheme: the invention provides a centrifugation-free pretreatment method for plant samples with magnetic particle-assisted solid-liquid rapid separation, which comprises the following steps: (1) Adding an extraction solvent into a plant samp