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Establishment of liquid chromatographic retention index and application of establishment to compound qualitative aspect

A retention index and liquid chromatography technology, which is applied in the establishment of liquid chromatography retention index and its application in the field of compound characterization, can solve the problems of lack of liquid chromatography retention index auxiliary qualitative and other problems, and achieve the improvement of identification reliability and standard The effect of unifying objects and assisting accurate qualitative

Active Publication Date: 2017-02-22
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a standard chromatographic analysis condition and the retention index of markers to assist in the qualitative analysis of complex sample components for the lack of liquid chromatography retention index in the prior art.

Method used

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  • Establishment of liquid chromatographic retention index and application of establishment to compound qualitative aspect
  • Establishment of liquid chromatographic retention index and application of establishment to compound qualitative aspect
  • Establishment of liquid chromatographic retention index and application of establishment to compound qualitative aspect

Examples

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Embodiment 1

[0034] Firstly, a mixed solution of retention index markers was prepared, and the markers were detected by LC-MS / MS under standard chromatographic conditions and their retention index values ​​were determined; fresh tobacco leaves were quick-frozen in liquid nitrogen, freeze-dried and pulverized.

[0035] Weigh 45-50 mg of freeze-dried fresh tobacco leaves (Safflower Dajinyuan grown in Dali, Yunnan) into a glass test tube, add 1 mL of extraction solvent (adding the retention index marker in advance) to the glass tube, and the retention index marker The concentration is 10ng mL -1 , put it in an ultrasonic cleaning machine after being sealed with a cover, ultrasonically extract in an ice bath for 30 min, the ultrasonic power is 100 Hz, and then centrifuge at 8000 rpm for 5 min, take the supernatant and filter it, and perform LC-MS / MS analysis, the resulting total ion current TIC is as follows image 3As shown, the names, precursor ions, product ions, collision energies and c...

Embodiment 2

[0039] Firstly, a mixed solution of retention index markers was prepared, and the markers were detected by LC-MS / MS under standard chromatographic conditions and their retention index values ​​were determined; fresh tobacco leaves were quick-frozen in liquid nitrogen, freeze-dried and pulverized.

[0040] Weigh 45-50 mg of freeze-dried fresh tobacco leaves (K326 planted in Zunyi, Guizhou) into a glass test tube, add 1 mL of extraction solvent (adding the retention index marker in advance) to the glass tube, the concentration of the retention index marker is 10 ngmL -1 , put it in an ultrasonic cleaning machine after being sealed with a cover, ultrasonically extract in an ice bath for 30 min, the ultrasonic power is 100 Hz, and then centrifuge at 8000 rpm for 5 min, take the supernatant and filter it, and perform LC-MS / MS analysis, the resulting total ion current TIC is as follows Figure 4 As shown, the names, precursor ions, product ions, collision energies and corrected re...

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Abstract

The invention provides establishment of the liquid chromatographic retention index and application of establishment to a compound qualitative aspect. Establishment specifically includes the following steps that firstly, a mixed solution of a retention index marker is prepared; secondly, under the standard chromatographic condition, LC-MS / MS detects the marker and determines the retention index value of the marker; thirdly, fresh tobacco leaves are quick-frozen with liquid nitrogen, freeze-dried and smashed; fourthly, the smashed sample is added into an extraction solvent and subjected to low-temperature ultrasonic extraction; fifthly, refrigerated centrifugation is conducted, and supernate is obtained and filtered; sixthly, LC-MS / MS detects the supermate and conducts qualitative analysis on a compound contained in the solution. Retention time of compound components in complex sample solutions can be corrected through the retention index marker, and retention time change caused by mobile phases, pressure or use of chromatographic columns different in batch number is avoided. Compared with the prior, multiple times of experiments under the same condition are not needed, the process is simple, cost is low, and qualitative accuracy and uniqueness can be greatly improved.

Description

technical field [0001] The invention relates to the establishment of liquid chromatography retention index in tobacco metabolomics research and its application in the qualitative aspect of compounds, specifically the establishment of standard chromatographic analysis conditions and the retention index of markers to assist in the qualitative analysis of complex sample components. Background technique [0002] In tobacco metabolomics research, the most important task is to accurately characterize compounds. In the past, the retention time was often used to compare with known substances. Generally, a pure product was used to identify a compound, and the conditions were exactly the same, so that the retention time of the chromatographic peaks could be the same substance. However, this method has a fatal flaw. It needs to know or reasonably guess the composition of the sample, and it can provide pure products. If it is an exploratory research or pure products are difficult to obt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 陈霞陈千思郑庆霞刘萍萍周会娜金立锋王燃张慧申晓晔李泽锋
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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