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Method for measuring alpha acid and beta acid in hop by ion pair chromatography

An ion-pair chromatography and hop technology, which is applied in the field of determination of α-acid and β-acid in hops, can solve the problems of inability to separate humulone and added humulone, large damage to the chromatographic column, etc., and achieve repeatability and recovery The effect of good efficiency and avoiding the use of strong acidic mobile phase

Active Publication Date: 2012-07-25
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the acidic condition is more damaging to the chromatographic column, and the humulone and adhumulone cannot be separated

Method used

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  • Method for measuring alpha acid and beta acid in hop by ion pair chromatography
  • Method for measuring alpha acid and beta acid in hop by ion pair chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Accurately weigh 0.0507 g of the hop extract sample, dissolve it with chromatographically pure methanol at a weight ratio of 400 times to constant volume, filter the obtained solution through a 0.25 μm organic phase filter membrane to remove insoluble substances, and inject the sample for analysis;

[0020] Liquid chromatography analysis conditions:

[0021] Chromatographic column: Zorbax SB-C18 analytical column (250mm×4.6mm, 5μm);

[0022] Mobile phase: the organic phase is methanol; the aqueous phase is 0.15M triethanolamine aqueous solution, and the pH is adjusted to 6.0 by phosphoric acid;

[0023] Gradient elution conditions: the initial organic phase ratio is 60%; the organic phase ratio reaches 80% after 40 minutes; the organic phase ratio increases to 100% after 50 minutes;

[0024] The injection volume is 10 μL, the flow rate is 0.8 mL / min, and the column temperature is 30 degrees Celsius;

[0025] Detection wavelength: the detection wavelength of the three ...

Embodiment 2

[0028] Take 1 mL of hop tincture, dilute it 5 times with chromatographically pure methanol, filter it through a 0.25 μm organic phase filter membrane, and inject it for analysis;

[0029] Liquid chromatography analysis conditions:

[0030] Chromatographic column: Zorbax SB-C18 analytical column (250mm×4.6mm, 5μm);

[0031] Mobile phase: the organic phase is methanol; the aqueous phase is 0.15M triethanolamine aqueous solution, and the pH is adjusted to 6.0 by phosphoric acid;

[0032] Gradient elution conditions: the initial organic phase ratio is 60%; the organic phase ratio reaches 80% after 40 minutes; the organic phase ratio increases to 100% after 50 minutes;

[0033] The injection volume is 10 μL, the flow rate is 0.8 mL / min, and the column temperature is 30 degrees Celsius;

[0034] Detection wavelength: the detection wavelength of the three α-acids is 328nm, and the detection wavelength of the three β-acids is 356nm.

[0035] The sample spectrum is shown in Figure-2...

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Abstract

The invention relates to a method for measuring alpha acid and beta acid in hops by an ion pair chromatography, which is characterized by comprising the following steps: a, preparing samples: preparing a hops tinctures sample by weighing a given weight of hops tinctures, diluting the hops tinctures with four to six times of chromatographic pure methanol in proportion by weight and filtering the diluted hops tinctures with 0.25 mu m of an organic phase filter membrane; preparing hops extractum by weighing a given weight of extraxtum, dissolving the hops extractum with 380-420 times of chromatographic pure methanol in proportion by weight and filtering the dissolved hops extrantum with 0.25 mu m of the filter membrane; and b, analyzing the prepared samples in step a by a diode-array detector of a liquid chromatogram. Compared with an original method for analyzing alpha acid and beta acid in hops, the method uses ion pair agent to avoid using strongly acid mobile phase, realizes better separation effect for alpha acid and beta acid than that of the current method, has good repeatability and recovery rate of experiments and is suitable for analysis of large quantities of samples.

Description

technical field [0001] The invention relates to a method for determining α-acid and β-acid in hops by ion-pair chromatography. The method uses triethanolamine as an ion-pairing reagent to realize the simultaneous determination of three kinds of α-acids and three kinds of β-acids in hop tincture under the condition of weakly acidic mobile phase. technical background [0002] Hops, also known as hops, hops, and hops, are important raw materials for brewing beer. They endow beer with a unique aroma and bitterness and increase the antiseptic ability of beer. Although hops are added in a small amount in beer production, their impact on the quality cannot be ignored. The composition of hops is very complex, and its main components include hop resin, hop essential oil, tannin, pectin, nitrogenous compounds and carbohydrates. The soft resin in hops is the main source of hop aroma and bitterness, and is divided into two types: α-acid and β-acid. α-acids mainly include humulone, co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/38
Inventor 郭吉兆胡斌张晓兵赵晓东丁丽于晶晶
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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