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Method for simultaneously measuring alpha-acids, beta-acids and iso-alpha-acids in hops

A technology of hops and detection wavelength, applied in the field of chemical analysis and detection, can solve the problems of repeated experimental operation, waste of time, etc., and achieve the effect of simple operation

Inactive Publication Date: 2014-01-08
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current detection methods for α-acids, β-acids and iso-α-acids are independent, and the experimental operation is repeated and wastes time
There is no detection method that can effectively analyze and determine 9 substances of 3 kinds of α-acids, 3 kinds of β-acids and 3 kinds of iso-α-acids at the same time, which saves time and can effectively separate

Method used

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  • Method for simultaneously measuring alpha-acids, beta-acids and iso-alpha-acids in hops
  • Method for simultaneously measuring alpha-acids, beta-acids and iso-alpha-acids in hops

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Accurately weigh a sample of hop extract, accurately weigh 0.1g, place it in a 50mL beaker, dissolve it with 40mL methanol, place in an ultrasonic water bath for 10-20min, transfer to a 100mL volumetric flask, dilute with methanol, and mix thoroughly. Filter with a 0.45μm organic filter membrane, store it in a sample bottle, and analyze it.

[0020] Analysis conditions of reversed-phase liquid chromatography:

[0021] Column: EC 250 / 4Nuclesoil 100-5C18

[0022] Elution conditions: mobile phase: organic phase B is acetonitrile; inorganic phase A contains phosphoric acid (85%) 0.1%, 0.2mM EDTANa 2 Aqueous solution. The present invention adopts a gradient elution method, and the elution procedure is: 0-30min, 0%B-60%B; 30-32min, 60%B-70%; 32-50min, 70%B-75%B; 50- 55min, 75%B-60%B.

[0023] The injection volume is 10μL, the flow rate is 1.0mL / min, and the column temperature is 30℃.

[0024] Detection wavelength: the detection wavelength of iso-α-acid is 270nm, the detection wavele...

Embodiment 2

[0027] Weigh 5.0 g of the granular hop sample ground into powder, place it in a 250 mL conical flask with stopper, extract with 20 mL of methanol and 80 mL of ether, shake in a constant temperature 20°C shaker for 30 minutes, add 40 mL of 0.1 mol / L hydrochloric acid solution, and then Shake for 30 minutes, and then separate into layers. Take 5mL of the upper ether layer, dilute to 50mL with methanol, fully uniform, filter with a 0.45μm organic filter membrane, store in a sample bottle, and sample for analysis.

[0028] Analysis conditions of reversed-phase liquid chromatography:

[0029] Column: EC 250 / 4Nuclesoil 100-5C18

[0030] Elution conditions: mobile phase: organic phase B is acetonitrile; inorganic phase A contains phosphoric acid (85%) 0.1%, 0.2mM EDTANa 2 Aqueous solution. The present invention adopts a gradient elution method, and the elution procedure is: 0-30min, 0%B-60%B; 30-32min, 60%B-70%; 32-50min, 70%B-75%B; 50- 55min, 75%B-60%B.

[0031] The injection volume is 1...

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Abstract

The invention discloses a method for simultaneously measuring alpha-acids, beta-acids and iso-alpha-acids in hops by reverse-phase high-performance chromatography. By the aid of the method, nine substances including three types of the alpha-acids, three types of the beta-acids and three types of the iso-alpha-acids can be simultaneously separated quickly and effectively. The method is characterized in that chromatographic conditions include that a chromatographic column is an EC 250 / 4Nucleosoil 100-5C18 chromatographic column, a flowing phase A is aqueous solution [containing 0.1% of phosphoric acids and 0.2mM of EDTANa2 (ethylene diamine tetraacetic acid disodium)], and a flowing phase B is acetonitrile. The flowing speed is 1.0mL / min, dual-wavelength detection UV (ultraviolet) waves have wavelengths of 270nm and 315nm, the temperature of the column is 30 DEG C, and the volume of an injected sample is 10 microliters. The method is used for monitoring change relation among the alpha-acids, the beta-acids and the iso-alpha-acids in the hops in a production process for heterogenous particles and heterogenous extract of the hops, and provides a theoretical reference for production technology. In addition, the method also can be used for researching dynamic variation of the alpha-acids and the iso-alpha-acids of the hops in a wort boiling process. Besides, the method has the advantages of good stability and repeatability, simplicity in operation, accuracy and reliability.

Description

Technical field [0001] The invention adopts reversed-phase high performance liquid chromatography to simultaneously detect the quantitative analysis method of α-acid, β-acid and iso-α-acid in hops, and realizes the detection of six main isomers of α-acid and β-acid in hops Simultaneous determination of three isomers in iso-α-acids. The invention belongs to the field of chemical analysis and detection technical background [0002] Hops are an important raw material for brewing beer, and its α-acid and β-acid are not only its main flavor substances, but also the main substances in hops for antibacterial and anti-microbial pollution. The quality of hops is one of the important factors that affect beer quality---taste, flavor and stability, and the most critical issue is the accurate determination and identification of the content of α-acid and β-acid in the hops and their freshness. α-acids mainly include three isomers of humulone, cohumulone, and adhumulone. β-acids mainly includ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 刘春凤周芸芸李崎王金晶李永仙郑飞云
Owner JIANGNAN UNIV