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Method for simultaneously detecting mercaptan and non-mercaptan sulfur-containing substances in beer and wort

A technology of mercaptan and wort, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem that the detection of low molecular mercaptan and high molecular mercaptan cannot be completed at the same time, so as to reduce the minimum detection limit and increase the volatility , Improve the effect of authenticity and reliability

Active Publication Date: 2015-03-18
TSINGTAO BREWERY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can only detect high-molecular mercaptans such as MBT, and cannot complete the detection of low-molecular thiols and high-molecular thiols at the same time, and generally temperamental laboratories are equipped with EI sources instead of CI sources.

Method used

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  • Method for simultaneously detecting mercaptan and non-mercaptan sulfur-containing substances in beer and wort
  • Method for simultaneously detecting mercaptan and non-mercaptan sulfur-containing substances in beer and wort
  • Method for simultaneously detecting mercaptan and non-mercaptan sulfur-containing substances in beer and wort

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Experimental program
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specific Embodiment approach

[0038] (1) Instruments: gas chromatography mass spectrometer SCIONTQ (Bruker, USA), solid phase microextraction autosampler Autosampler (Bruker, USA).

[0039] (2) Reagents: methyl thioacetate (99%), ethyl thioacetate (99%), ethyl 3-methylthiopropionate (95%), 3-methylthiopropanol (98%) Dimethyl disulfide (95%), Dimethyl trisulfide (99%), Methyl mercaptan (99%), Ethyl mercaptan (98%), 3-Methyl-2-butene-1-mercaptan (95%), Benzylthiol 99% (Sigma, USA), PFBBr (99%), EDTA (analytical pure AR) (Shanghai Reagent No. 1 Factory).

[0040] Standard curve formulation:

[0041] Quantitative analysis is calibrated by the instrument with a standard substance. The standard substance is made into an aqueous solution and adjusted to a pH = 4 and an alcohol content of 5% similar to beer and wort. The prepared solution is used to prepare the concentration standard solution in Table 3. Get the calibration curve.

[0042] Table 3. Standard curve concentrations (unit: ng / L) and method validatio...

Embodiment 1

[0046] (1) Exhaust the wort sample, take 5mL and put it into a 20mL headspace bottle;

[0047] (2) Add 2g NaCl to the headspace bottle;

[0048] (3) Add 0.025g EDTA (disodium ethylenediamine tetraacetate) to the headspace bottle;

[0049] (4) Insert the 65 μm PDMS / DVB fiber extraction head into the headspace bottle filled with pentafluorobenzyl bromide (PFBBr) derivative liquid for 10 minutes to make the derivative liquid adsorb on the fiber extraction head; insert the fiber extraction head with PFBBr Derivative extraction was carried out in the headspace bottle containing the test sample, the extraction temperature was 55°C, and the extraction time was 10 minutes;

[0050] (5) After the extraction is completed, insert the fiber extraction head into the GC inlet, desorb for 2 minutes and enter the GC-MS / MS detection; the detection conditions of GC-MS / MS are as follows:

[0051] The chromatographic conditions are as follows: the gas chromatography column is DB-5MS, 0.25mm inn...

Embodiment 2

[0060] (1) Exhaust the beer sample, take 5mL and put it into a 20mL headspace bottle;

[0061] (2) Add 2g NaCl to the headspace bottle;

[0062] (3) Add 0.01g EDTA (disodium ethylenediamine tetraacetate) to the headspace bottle;

[0063] (4) Insert the 65 μm PDMS / DVB fiber extraction head into the headspace bottle filled with pentafluorobenzyl bromide (PFBBr) derivative liquid for 10 minutes to make the derivative liquid adsorb on the fiber extraction head; insert the fiber extraction head with PFBBr Derivative extraction was carried out in the headspace bottle containing the test sample, the extraction temperature was 55°C, and the extraction time was 10 minutes;

[0064] (5) After the extraction is completed, insert the fiber extraction head into the GC inlet, desorb for 2 minutes and enter the GC-MS / MS detection; the detection conditions of GC-MS / MS are as follows:

[0065] The chromatographic conditions are as follows: the gas chromatography column is DB-5MS, 0.25mm inne...

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Abstract

The invention discloses a method for simultaneously detecting mercaptan and non-mercaptan sulfur-containing substances in beer and wort. In the method, a headspace derivation solid phase microextraction-GCMS / MS (Gas Chromatography Mass Spectrometry / Mass Spectrometry) method is adopted to carry out detection; PFBBr is used as a derivatization reagent; in the extraction process, NaCl and EDTA (Ethylene Diamine Tetraacetic Acid) are added and an extraction head adsorbing the sulfur-containing substances is analyzed, separated and detected by GC-MS / M. According to the invention, due to change of the adsorption characteristic of the fiber extraction head, the fiber extraction head which cannot effectively extract trace mercaptan such as MBT (rubber accelerator) and the like implements simultaneous derivation and extraction of a volatile non-mercaptan sulfur-containing compound and mercaptan derivatives in beer and wort volatile matter so as to fulfill the aim of simultaneously detecting the non-mercaptan sulfur-containing compound and the mercaptan substance. According to the invention, five steps of adsorption of a derivative agent, derivation, extraction, sample injection, separation and detection can be sequentially completed in the same process; automatic continuous operation is implemented; detection efficiency and accuracy are improved; accurate and efficient quantitative analysis on the non-mercaptan sulfur-containing substance and the mercaptan substance in ten types of beer and wort is implemented.

Description

technical field [0001] The invention relates to an analysis and detection method for beer, in particular to a method for simultaneous detection of mercaptan and non-mercaptan sulfur-containing substances in beer and wort. Background technique [0002] Sulfur compounds in beer are a double-edged sword for beer flavor. When the value is lower than the threshold, they are indispensable substances for the flavor of beer, and when the value is higher than the threshold, they will have an adverse effect on the flavor of beer. Along with the change of consumer's taste, the day by day prevailing of light refreshing type beer, people are more and more sensitive to the sensation of the bad flavor substance in beer. Therefore, understanding the sulfur compounds in beer and taking effective measures to reduce the sulfur compounds in beer is one of the keys to brewing beer with excellent flavor. There are dozens of sulfur-containing volatile compounds in beer, and there are more than a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 尹花董建军陈华磊郝俊光闫鹏田玉红李华李梅杨朝霞张宇昕
Owner TSINGTAO BREWERY