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A method for fully automatic tandem solid-phase extraction of brassinosteroids in plants

A tandem solid-phase extraction and brassinosteroid technology, applied in the field of analytical chemistry, can solve problems such as large sample loss, and achieve the effects of reducing analysis costs, reducing matrix effects, and extremely high sample utilization.

Active Publication Date: 2021-04-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a fully automatic plant sample pretreatment method, which uses a fully automatic online solid phase extraction device to perform tandem solid phase extraction, purifies and enriches brassinosterol in complex plant samples, and improves the efficiency of subsequent chromatographic analysis. Selectivity and sensitivity, to solve the problem of large sample loss in the traditional offline sample pretreatment process

Method used

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  • A method for fully automatic tandem solid-phase extraction of brassinosteroids in plants
  • A method for fully automatic tandem solid-phase extraction of brassinosteroids in plants
  • A method for fully automatic tandem solid-phase extraction of brassinosteroids in plants

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Embodiment approach 1

[0032]A fully automatic online solid phase extraction device is used for solid phase extraction. The fully automatic online solid phase extraction device has two sets of pressure heads, which respectively clamp the solid phase extraction column A and the solid phase extraction column B. Solid phase extraction column A and solid phase extraction column B are cylinders, along the central axis of the column, there is a circular through hole running through the upper and lower ends. The diameter of the through hole is 1mm ~ 3mm, and the through hole is filled with solid adsorbent; the column The upper and lower ends are equipped with sieve plates that are tightly combined with the column to seal the filler in the through hole; the two ends of the solid phase extraction column A and the solid phase extraction column B are comparable in size to the pressure head of the automatic online solid phase extraction device. match. Solid-phase extraction column A is filled with C8 or C18 bon...

Embodiment approach 2

[0038] The difference from Embodiment 1 is that a derivation reaction tube is connected between positions ② and ⑤ of the six-way valve for online derivation of brassinosterol. The derivatization reaction tube is a quartz coil tube with an inner volume of 100 microliters to 300 microliters. The ③ position of the six-way valve is the mobile phase inlet, and the ④ position is connected to the chromatographic column. At this time, the ④ position of the six-way valve in the steps a, b and c is connected to the ③ position; The ⑧ position enters, and flows through the solid phase extraction column A and the solid phase extraction column B in sequence, and the brassinosterol is eluted and brought into the derivatization reaction tube to stop flow for 20s~60s for derivatization; the derivatization liquid contains derivatization reagent and 5% to 10% (v / v) pyridine in acetonitrile solution; after the derivatization reaction is finished, perform step d, switch the eight-way valve and th...

Embodiment 1

[0041] A full-automatic online solid-phase extraction device is used to carry out solid-phase extraction on the rice sample extract. The full-automatic online solid-phase extraction device has two sets of pressure heads, which respectively clamp the solid-phase extraction column A and the solid-phase extraction column B. Solid phase extraction column A and solid phase extraction column B are cylinders, along the central axis of the column, there is a circular through hole running through the upper and lower ends. The diameter of the through hole is 2.5mm, and the through hole is filled with solid adsorbent; Both ends are provided with a sealing sieve plate tightly combined with the column to seal the filler in the through hole; the outer diameter of the solid phase extraction column A and solid phase extraction column B is comparable to the pressure head size of the automatic online solid phase extraction device. match. Solid-phase extraction column A was filled with 40 μL C18...

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Abstract

The invention discloses a pre-analysis method for the analysis of brassinosterol in plants by using a fully automatic tandem solid-phase extraction method. The method adopts a fully automatic online solid phase extraction device, and connects two solid phase extraction columns in series to purify and purify plant sample extracts online, and it is used in conjunction with chromatographic sampling online, which solves the problem of sample loss in the traditional offline sample pretreatment process Bigger problem. The online series use of the two solid phase extraction columns can improve the purification efficiency, reduce the matrix effect of chromatographic analysis, and improve the analysis selectivity. At the same time, the two solid-phase extraction columns can be regenerated online after use, and can be reused many times, which reduces the analysis cost and saves analysis time. The method also integrates an online derivatization function, which is beneficial to improve the detection sensitivity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a pretreatment method for plant samples, which is suitable for sample pretreatment when analyzing brassinosteroids in plant samples. Background technique [0002] Quantitative detection of trace phytohormones in plants has always been an analytical challenge in botany research. Among them, brassinosterol has attracted much attention because of its high activity. Due to the complex matrix of plant samples, the content of brassinosterol is extremely low (generally, the content in buds and leaves is only about 0.01-0.1ng / g fresh weight), so efficient sample pretreatment methods are required to remove a large amount of impurities and enrich brassinosterol. In the prior art, a combination of liquid phase extraction, solid phase extraction (solid phase extraction, SPE), matrix solid phase dispersion (matrix solid phase dispersion, MSPD) and other methods is often used t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08G01N30/02
CPCG01N30/02G01N30/08G01N2030/062
Inventor 段春凤关亚风李玉璇倪兰秀
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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