CN112730669A - Method for measuring cinnamaldehyde, eugenol, carvacrol and thymol - Google Patents

Method for measuring cinnamaldehyde, eugenol, carvacrol and thymol Download PDF

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Publication number
CN112730669A
CN112730669A CN202011535938.5A CN202011535938A CN112730669A CN 112730669 A CN112730669 A CN 112730669A CN 202011535938 A CN202011535938 A CN 202011535938A CN 112730669 A CN112730669 A CN 112730669A
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CN
China
Prior art keywords
solution
measuring
carvacrol
eugenol
cinnamaldehyde
Prior art date
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Pending
Application number
CN202011535938.5A
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Chinese (zh)
Inventor
凌满
陈立萍
王腾浩
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Zhejiang Gaosheng Biotechnology Co ltd
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Zhejiang Gaosheng Biotechnology Co ltd
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Priority to CN202011535938.5A priority Critical patent/CN112730669A/en
Publication of CN112730669A publication Critical patent/CN112730669A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/30Control of physical parameters of the fluid carrier of temperature
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/32Control of physical parameters of the fluid carrier of pressure or speed
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/34Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/74Optical detectors
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/32Control of physical parameters of the fluid carrier of pressure or speed
    • G01N2030/324Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a method for measuring cinnamaldehyde, eugenol, carvacrol and thymol, belonging to the field of detection, and the method for measuring cinnamaldehyde, eugenol, carvacrol and thymol comprises the following steps: a. preparing a measuring solution; weighing 0.5g-1g (accurate to 0.0001g) of sample in a 50mL volumetric flask, adding 30mL of methanol, performing ultrasonic treatment for 20-30min, and fixing the volume of the methanol to the scale of the volumetric flask; b. solution dilution: diluting the prepared solution with deionized water; c. filtering the solution: passing the diluted solution through a filter membrane to obtain a test sample solution; d. liquid chromatography determination: injecting the prepared sample solution and the standard working solution into a liquid chromatograph for measurement; e. content determination: calculating the content of effective components in the sample by using a peak height external standard method; the invention can directly extract four different components in the plant essential oil, directly measure by a liquid chromatograph, and has simple and rapid operation and high efficiency.

Description

Method for measuring cinnamaldehyde, eugenol, carvacrol and thymol
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a determination method of cinnamaldehyde, eugenol, carvacrol and thymol.
Background
Plant essential oil is widely used in the feed industry as one of the substitute antibiotics in the animal husbandry at present. The plant essential oil has good antibacterial activity, palatability and growth promoting effect, and can be used as a good antibiotic substitute. Cinnamaldehyde, eugenol, carvacrol and thymol are used as a plurality of commonly used plant essential oil components, most of the detection methods are gas chromatography, and liquid chromatography is rarely used, or one or two components are detected by the liquid chromatography, and no four components are detected by the liquid chromatography together temporarily. The invention aims to solve the problem of liquid chromatography detection of four components.
Disclosure of Invention
The invention aims to provide a method for measuring cinnamaldehyde, eugenol, carvacrol and thymol.
In order to achieve the purpose, the invention provides the following technical scheme: a method for measuring cinnamaldehyde, eugenol, carvacrol and thymol comprises the following steps:
a. preparing a measuring solution; weighing 0.5g-1g (accurate to 0.0001g) of sample in a 50mL volumetric flask, adding 30mL of methanol, performing ultrasonic treatment for 20-30min, and fixing the volume of the methanol to the scale of the volumetric flask;
b. solution dilution: diluting the prepared solution with deionized water;
c. filtering the solution: passing the diluted solution through a filter membrane to obtain a test sample solution;
d. liquid chromatography determination: injecting the prepared sample solution and the standard working solution into a liquid chromatograph for measurement;
e. content determination: and calculating the content of the effective components in the sample by using a peak height external standard method.
Preferably, when the solution is diluted, the solution is diluted to the concentration of the standard curve of the four components of the cinnamaldehyde, the eugenol, the carvacrol and the thymol, wherein the lowest standard concentration range.
Preferably, the filter membrane is a 0.45 μm size filter membrane.
Preferably, when the measurement is carried out by a liquid chromatograph, the measurement is carried out according to the following chromatographic conditions:
a chromatographic column: c18 column, 150mm × 4.6mm, particle size 5 μm.
Mobile phase: acetonitrile + water-40 + 60.
Detection wavelength: 280 nm.
Column temperature: at 40 ℃.
Flow rate: 1.0 ml/min.
Sample introduction amount: 20 μ L.
The invention has the beneficial effects that:
1. the liquid chromatograph is used for detecting the four components of the cinnamyl aldehyde, the eugenol, the carvacrol and the thymol in the plant essential oil, and the liquid chromatograph is used as a stock instrument in the feed industry, so that the use cost is low, the four different components in the plant essential oil are directly extracted, the measurement is directly carried out by the liquid chromatograph, the operation is simple and rapid, and the efficiency is high.
2. The method has simple sample pretreatment process and greatly improves the operation efficiency.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following examples are given.
The measuring methods of cinnamaldehyde, eugenol, carvacrol and thymol according to the examples of the present invention will be described in detail below.
The method for measuring the cinnamaldehyde, the eugenol, the carvacrol and the thymol comprises the following steps:
sample processing
Weighing 0.5g-1g (accurate to 0.0001g) sample in a 50mL volumetric flask, adding 30mL methanol, performing ultrasonic treatment for 20-30min, and metering the volume of the methanol to the scale of the volumetric flask.
Measurement sample preparation
Diluting the prepared solution with deionized water to the concentration of standard curves of the four components of cinnamaldehyde, eugenol, carvacrol and thymol, wherein the concentration is within the lowest standard concentration range; the diluted solution was passed through a filter membrane of 0.45 μm size to obtain a test sample solution.
Liquid chromatography assay
The following chromatographic conditions were used:
a chromatographic column: c18 column, 150mm × 4.6mm, particle size 5 μm.
Mobile phase: acetonitrile + water-40 + 60.
Detection wavelength: 280 nm.
Column temperature: at 40 ℃.
Flow rate: 1.0 ml/min.
Sample introduction amount: 20 mu L of the solution;
and injecting the prepared sample solution and the standard working solution into a liquid chromatograph for measurement.
Determination of component content
And calculating the content of the effective components in the sample by using a peak height external standard method.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. A method for measuring cinnamaldehyde, eugenol, carvacrol and thymol is characterized by comprising the following steps:
a. preparing a measuring solution; weighing 0.5g-1g (accurate to 0.0001g) of sample in a 50mL volumetric flask, adding 30mL of methanol, performing ultrasonic treatment for 20-30min, and fixing the volume of the methanol to the scale of the volumetric flask;
b. solution dilution: diluting the prepared solution with deionized water;
c. filtering the solution: passing the diluted solution through a filter membrane to obtain a test sample solution;
d. liquid chromatography determination: injecting the prepared sample solution and the standard working solution into a liquid chromatograph for measurement;
e. content determination: and calculating the content of the effective components in the sample by using a peak height external standard method.
2. The method for measuring cinnamaldehyde, eugenol, carvacrol and thymol according to claim 1, wherein the dilution of the solution is performed to a concentration within a standard curve of four components of cinnamaldehyde, eugenol, carvacrol and thymol, wherein the concentration is within the lowest standard concentration range.
3. The method for measuring cinnamaldehyde, eugenol, carvacrol and thymol according to claim 1, wherein the filter membrane is a 0.45 μm size filter membrane.
4. The method for measuring cinnamaldehyde, eugenol, carvacrol and thymol according to claim 1, wherein the measurement is performed by a liquid chromatograph under the following chromatographic conditions:
a chromatographic column: c18 column, 150mm × 4.6mm, particle size 5 μm.
Mobile phase: acetonitrile + water-40 + 60.
Detection wavelength: 280 nm.
Column temperature: at 40 ℃.
Flow rate: 1.0 ml/min.
Sample introduction amount: 20 μ L.
CN202011535938.5A 2020-12-23 2020-12-23 Method for measuring cinnamaldehyde, eugenol, carvacrol and thymol Pending CN112730669A (en)

Priority Applications (1)

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CN202011535938.5A CN112730669A (en) 2020-12-23 2020-12-23 Method for measuring cinnamaldehyde, eugenol, carvacrol and thymol

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CN202011535938.5A CN112730669A (en) 2020-12-23 2020-12-23 Method for measuring cinnamaldehyde, eugenol, carvacrol and thymol

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113777196A (en) * 2021-09-13 2021-12-10 天津春发生物科技集团有限公司 Method for simultaneously determining six spicy components in solid food by DAD-HPLC

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020107287A1 (en) * 1999-04-29 2002-08-08 Bessette Steven M. Pesticidal activity of plant essential oils and their constituents
CN102014616A (en) * 2008-03-19 2011-04-13 蒂拉德克公司 Pest control using natural pest control agent blends
CN107843676A (en) * 2017-11-15 2018-03-27 广州美瑞泰科生物工程技术有限公司 The detection method of carvacrol and Thymol in a kind of plant extract feed additive

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020107287A1 (en) * 1999-04-29 2002-08-08 Bessette Steven M. Pesticidal activity of plant essential oils and their constituents
CN102014616A (en) * 2008-03-19 2011-04-13 蒂拉德克公司 Pest control using natural pest control agent blends
CN107843676A (en) * 2017-11-15 2018-03-27 广州美瑞泰科生物工程技术有限公司 The detection method of carvacrol and Thymol in a kind of plant extract feed additive

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
任玉琴 等: "高效液相色谱法同时测定饲料香味剂中肉桂醛、丁香酚、香芹酚和百里香酚含量的研究", 《中国饲料》 *
张玮 等: "高效液相色谱法测定混合型饲料添加剂中肉桂醛、丁香酚、香芹酚和百里香酚含量", 《饲料研究》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113777196A (en) * 2021-09-13 2021-12-10 天津春发生物科技集团有限公司 Method for simultaneously determining six spicy components in solid food by DAD-HPLC

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