A method for the separation and detection of coniferyl alcohol and sinapyl alcohol by gas chromatography

A gas chromatography-mass spectrometry and coniferyl alcohol technology, which is applied in material separation, measuring device, analyzing materials, etc., can solve the problems of less research on coniferyl alcohol and sinapyl alcohol, no separation and detection methods, etc., and achieves easy implementation, good application prospect, and simple process. Effect

Active Publication Date: 2018-12-18
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Coniferyl alcohol and sinapyl alcohol belong to phenolic alcohol compounds. The boiling point of coniferyl alcohol is 163-165°C, and the boiling point of sinapyl alcohol is 384.7°C. The boiling point of coniferyl alcohol and sinapyl alcohol is relatively low under normal pressure. In addition, there are few studies on coniferyl alcohol and sinapyl alcohol. The commonly used NIST library There is no derivatized structure of coniferyl alcohol and sinapyl alcohol, and there is no suitable separation and detection means in the prior art, so there is an urgent need for a method that can effectively separate and detect coniferyl alcohol and sinapyl alcohol

Method used

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  • A method for the separation and detection of coniferyl alcohol and sinapyl alcohol by gas chromatography
  • A method for the separation and detection of coniferyl alcohol and sinapyl alcohol by gas chromatography
  • A method for the separation and detection of coniferyl alcohol and sinapyl alcohol by gas chromatography

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Embodiment 1

[0028] A method for separating and detecting coniferyl alcohol and sinapyl alcohol by gas chromatography, comprising the following steps:

[0029] (1) Preparation of the test product

[0030] (a) Accurately weigh 0.0010 mg coniferyl alcohol and 0.0010 mg sinapyl alcohol using an analytical balance;

[0031] (b) The weighed coniferyl alcohol and sinapyl alcohol were dissolved in 2mL chromatographic grade pyridine respectively to obtain a coniferyl alcohol standard solution and a sinapyl alcohol standard solution;

[0032] (c) Take 100 μL coniferyl alcohol standard solution and 100 μL sinapyl alcohol standard solution respectively, and then carry out derivatization treatment respectively. The specific process of derivatization treatment is: add 60 μL hydroxylamine hydrochloride pyridine solution (20mg hydroxylamine hydrochloride / mL pyridine, the same below ), vortexed for 60s, then oximated at 100°C for 2h, then added 60μL of BSTFA+TMCS (99:1) silylating reagent, vortexed for 6...

Embodiment 2

[0041] A method for separating and detecting coniferyl alcohol and sinapyl alcohol by gas chromatography, comprising the following steps:

[0042] (1) Preparation of the test product

[0043] (a) Accurately weigh 0.0010 mg coniferyl alcohol and 0.0010 mg sinapyl alcohol using an analytical balance;

[0044] (b) Dissolve the weighed coniferyl alcohol and sinapyl alcohol in 4mL chromatographic grade pyridine to obtain a mixed standard solution;

[0045] (c) Take 100 μL of mixed standard solution, and then perform derivatization treatment. The specific process of derivatization treatment is: add 50 μL of hydroxylamine pyridine hydrochloride solution, vortex for 30 seconds, and then oximate at 100°C for 1.5 hours, then add 50 μL BSTFA+TMCS (99:1) silanization reagent, vortex for 30s, and finally silanization at 100°C for 1.5h to obtain a mixed sample to be tested;

[0046] (2) Separation and detection of the test product

[0047] Use gas chromatography-mass spectrometry to sepa...

Embodiment 3

[0054] A method for separating and detecting coniferyl alcohol and sinapyl alcohol by gas chromatography, comprising the following steps:

[0055] (1) Preparation of the test product

[0056] (a) Accurately weigh 0.0010 mg coniferyl alcohol and 0.0010 mg sinapyl alcohol using an analytical balance;

[0057] (b) Dissolve the weighed coniferyl alcohol and sinapyl alcohol in 4mL chromatographic grade pyridine to obtain a mixed standard solution;

[0058] (c) Take 100 μL of the mixed standard solution, and then perform derivatization treatment. The specific process of derivatization treatment is: add 70 μL of hydroxylamine pyridine hydrochloride solution, vortex for 45 seconds, and then oximate at 100°C for 2.5 hours, then add 70 μL BSTFA+TMCS (99:1) silanization reagent, vortex for 45s, and finally silanization at 100°C for 2.5h to obtain a mixed sample to be tested;

[0059] (2) Separation and detection of the test product

[0060] Use gas chromatography-mass spectrometry to ...

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Abstract

The invention discloses a method for separating and detecting coniferyl alcohol and sinapyl alcohol through gas chromatography-mass spectrometry (GC-MS). The method comprises the following steps: (1) dissolving a sample containing coniferyl alcohol and / or sinapyl alcohol in chromatographic grade pyridine to obtain a sample solution and then carrying out derivatization treatment on the sample solution, thus obtaining a sample to be detected; (2) separating and detecting the sample to be detected obtained in the step (1) through GC-MS. The method applying GC-MS can be used for effectively separating and detecting coniferyl alcohol and sinapyl alcohol, has the effects of determining the retention time and main ion peaks of coniferyl alcohol and sinapyl alcohol, filling up the structure gaps after derivatization of coniferyl alcohol and sinapyl alcohol in the NIST database and constructing the GC-MS detection mass spectrum after derivatization of coniferyl alcohol and sinapyl alcohol, can be used for separating and detecting coniferyl alcohol and sinapyl alcohol, has high detection accuracy, is simple in process, is easy to implement and has a very good application prospect.

Description

technical field [0001] The invention relates to the field of substance separation and detection, in particular to a method for separation and detection of coniferyl alcohol and sinapyl alcohol by gas chromatography. Background technique [0002] Both coniferyl alcohol and sinapyl alcohol are less researched chemical substances, and the structural formula of coniferyl alcohol is shown in the appendix of the description. figure 1 , the structural formula of sinapyl alcohol is shown in the appendix figure 2 , many of their physicochemical properties are unknown, and they are key intermediate metabolites in the lignin metabolic pathway. Studying coniferyl alcohol and sinapyl alcohol is conducive to better research on metabolic pathways. [0003] Coniferyl alcohol and sinapyl alcohol belong to phenolic alcohol compounds. The boiling point of coniferyl alcohol is 163-165°C, and the boiling point of sinapyl alcohol is 384.7°C. The boiling point of coniferyl alcohol and sinapyl a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/067
Inventor 蔡永萍李姝妹金青林毅张金云程曦曹运鹏余诚峰
Owner ANHUI AGRICULTURAL UNIVERSITY
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