CN103675126B - Purge-and-trap detection method of volatile flavor substances in sour-dough steamed bun - Google Patents

Purge-and-trap detection method of volatile flavor substances in sour-dough steamed bun Download PDF

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CN103675126B
CN103675126B CN201310613183.XA CN201310613183A CN103675126B CN 103675126 B CN103675126 B CN 103675126B CN 201310613183 A CN201310613183 A CN 201310613183A CN 103675126 B CN103675126 B CN 103675126B
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purge
steamed bun
trap
sour
temperature
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CN103675126A (en
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何国庆
张国华
朱永胜
何捷
刘同杰
陈启和
阮辉
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a purge-and-trap detection method of volatile flavor substances in a sour-dough steamed bun. The method comprises the steps as follows: after the sour-dough steamed bun is cooled and diced, a purge-and-trap device is adopted to collect the volatile flavor substances; and a gas chromatography-mass spectrometry technology is adopted to evaluate the volatile flavor substances. According to the method, an organic solvent is not required, the sampling quantity is small, the enrichment efficiency is high, matrix interference is little, trace component loss can be effectively reduced, and the detection rate of trace components is increased.

Description

The purge and trap detection method of volatile flavor substance in sour flour dough steamed bun
Technical field
The present invention relates to fermented food local flavor analysis technical field, particularly relate to the purge and trap detection method of volatile flavor substance in a kind of sour flour dough steamed bun.
Background technology
Steamed bun (Chinese Steamed Bread), also referred to as steamed bun or steamed bun, is the traditional staple food originating from China, in China particularly northern area daily life, occupies critical role.According to statistics, the annual steamed bun of northern China account for about 70% of flour total amount by powder amount.Steamed bun is mainly raw material with wheat flour, add water, yeast or leaven (leavening dough, leaven, bottle opener, old face) etc. with become dough fermentation, through the kneading, shaping and the process such as to proof of dough, eventually passing decatize slaking is finished product.
Sour flour dough steamed bun, refers to the fermented dough with cooking steamed bun last time and staying, and in this, as leaven, adds flour and becomes dough and ferment, add appropriate bases, and face aftershaping, proofs and steams steamed bun.China is as far back as just bringing into use sour flour dough fermenting and producing steamed bun 13rd century.Enter China market along with namely 20th century the mid-80 sends out active dry yeast, the advantages such as because active dry yeast activity is high, fermenting power is large, and use amount is few, so people start to steam steamed bun with active dry yeasr.Because dry ferment is pure-blood ferment, the steamed bun local flavor made is dull, and traditional zymotic sour flour dough is the Tiny ecosystem system of multiple-microorganism symbiosis, it is the synergy of multiple-microorganism saccharification, fermentation, esterification, institutional framework is more tending towards soft fine and smooth and whippy mouthfeel, and generates the multiple flavor substances such as alcohol, ester, aldehyde, phenol, acid, low molecular sugar, polypeptide, amino acid.So the steamed bun quality made is careful, unique flavor, enjoys the favor of consumers in general.
The principal ingredient of its part fragrance of sour flour dough steamed bun flavor substance complicated component is trace components, the detection method that current trace components is conventional is: direct injected Gc-ms, solid-phase microextraction Gc-ms, purging/trapping-thermal desorption low-polarity components etc., and wherein purging/trapping-thermal desorption low-polarity components is the technology of a kind of comparatively novel sample pre-treatments and compartment analysis desired combination.Purge and trap technology is dynamic headspace analysis technology, different from Static Headspace, Dynamic headspace is not the headspace sample analyzing equilibrium state, but with flowing gas by the volatile ingredient " purging " in sample out, with a drip catcher, the species adsorbs of producing by boasting is got off again, then through thermal desorption, sample is sent into GC and analyze.Therefore, purging is commonly referred to--trapping (Purge & Trap) sampling technique.
Purge in the overwhelming majority--all adopt helium as sweep gas in trapping application, by it with passing into sample solution bubbling.Under the gas flow purging continued, the volatile constituent in sample is overflowed with helium, and is concentrated by a capturing device that adsorbent is housed.After certain purge time, survey component is waited all or quantitatively to enter drip catcher.Now, shut-down purge gas, that drip catcher accessed GC by transfer valve opens gas gas circuit, enters GC compartment analysis after the sample component desorb of Fast Heating trapping simultaneously with carrier gas.So, purging--the principle of trapping is exactly: Dynamic headspace extraction-adsorbing and trapping thermal desorption-GC analyzes.Puffing and trapping without the need to an organic solvent, does not cause secondary pollution to environment to the pre-treatment of sample, and have that sampling amount is few, bioaccumulation efficiency is high, little and easily realize the advantages such as on-line checkingi by Matrix effects.
Purge & trap sampling technique is widely used in environmental analysis, as the organic pollutant analysis in potable water or waste water.Also for the analysis of volatile matter in food (as odour component), but volatile flavor substance in report employing purge and trap technical Analysis sour flour dough steamed bun is had not yet to see.
Summary of the invention
The invention provides the purge and trap detection method of volatile flavor substance in a kind of sour flour dough steamed bun, without the need to an organic solvent, sampling amount is few, bioaccumulation efficiency is high, little by Matrix effects, effectively can reduce the loss of trace components, improve trace components recall rate.
A purge and trap detection method for volatile flavor substance in sour flour dough steamed bun, comprising:
(1) by after the cooling of sour flour dough steamed bun, stripping and slicing, scavenging trap is adopted to collect volatile flavor substance;
(2) gas chromatography-mass spectrometry analysis technology is adopted to identify described volatile flavor substance.
Purging/trapping-thermal desorption method is adopted to carry out pre-treatment to sample, can each component effectively in enriched sample, then gas chromatography-mass spectrometry analysis, accurately can detect the volatile compound in sample.
In step (1), the cool time of described sour flour dough steamed bun can be 5-10min, is convenient to steamed bun stripping and slicing.
After described sour flour dough steamed bun stripping and slicing, particle diameter is 50-100 order, is convenient to extraction.
Described scavenging trap can be the full-automatic scavenging trap of Tekmar Atomx.
The treatment conditions of described scavenging trap: purging temperature is 40-45 DEG C, purge time is 50-60min, and purge flow rate is 25-30mL/min, and dry blowing temp is 20-25 DEG C, dryly blows time 2-3min, and dry wind drift speed is 100-110mL/min.
Preferably, the treatment conditions of described scavenging trap: purging temperature is 40 DEG C, and purge time is 50min, and purge flow rate is 25mL/min, and dry blowing temp is 20 DEG C, dryly blows time 2min, and dry wind drift speed is 100mL/min.Impact purges the factor of efficiency and mainly contains and purge temperature, the flow velocity of sweep gas and flow, trapping time etc.Improve and purge temperature, be equivalent to improve vapour pressure, therefore purge efficiency and also can improve, but the spinoff of raised temperature adds the volatilization of water.By test, determine that purging temperature is 40 DEG C.Sweep gas flow velocity depend on the concentration of determinand in sample, volatility, with the interaction (as solubleness) of sample substrate and its suction-operated size in trap tube.Purging flow velocity can affect the trapping of sample time too large, cause the loss of sample component.By test, determine that purge flow rate is 25mL/min.Purge time is one of important parameter of purge & trap technology, must optimize determine according to concrete sample.In principle, purge time is longer, analyze reappearance and sensitivity higher.But consider analysis time and work efficiency, under satisfied analysis requires prerequisite, purge time short as far as possible should be selected.By test, determine that purge time is 50min.
In step (2), during gas chromatographic analysis, Agilent7890A-Agilent7000 gas chromatography mass spectrometry instrument can be adopted, DB-WAX(30m × 0.25mm × 0.25 μm) capillary chromatographic column, with Splitless injecting samples, carrier gas done by helium, and flow rate of carrier gas is 0.8 ~ 1.2mL/min, and injector temperature is 230 ~ 250 DEG C.
During gas chromatographic analysis, adopt following temperature programme: initial temperature 40 DEG C, keep 3min, be warming up to 200 DEG C with 5 DEG C/min, then be warming up to 230 DEG C with 10 DEG C/min, keep 3min.
Mass spectrophotometry condition can be: ionization mode is EI, ionization voltage 70eV, filament emission current 35 μ A, ion source temperature 230 DEG C, and interface temperature 280 DEG C, detection mode is full ion scan.
Described sour flour dough steamed bun can be prepared by the following method:
(1) sour flour dough is added to the water immersion, adds wheat flour after having soaked, mixing, is placed in temperature 28-32 DEG C, relative humidity 70-80% condition bottom fermentation 2.5-4h;
(2) after having fermented, add wheat flour and water, then carry out kneading dough, split, rub circle, shaping with the hands, then be placed in temperature 28-32 DEG C, proof 40-70min under relative humidity 70-80% condition;
(3) after having proofed, steam, obtain sour flour dough steamed bun.
Wherein, in step (1), in every kilogram of sour flour dough, described immersion water consumption is 0.3-0.5kg, and the addition of wheat flour is 0.6-0.9kg; In step (2), in every kilogram of sour flour dough, the addition of described wheat flour is 1.1-1.4kg, and the addition of water is 0.5-0.8kg.
Adopt the sour flour dough steamed bun of above method, mouthfeel is good, and institutional framework is soft fine and smooth, and flavor substance kind is many, nutritious.
The present invention carries out enrichment by using purge and trap pretreatment technology to the flavor substance of sour flour dough steamed bun, compared with Static Headspace, purge and trap technology can analyze low-molecular-weight volatility and semi-volatile compounds, stronger to the identification and analysis ability of alcohols and aldehyde compound, and do not need to use solvent extraction, not causing secondary pollution to environment, is a kind of eco-friendly technology, can eliminate operating personnel and be exposed to proemial chemicals and without the need to carrying out refuse process to solvent; And sampling amount is few, simple to operate, environmental friendliness, little by Matrix effects, bioaccumulation efficiency is high, highly sensitive, automaticity is high, easily realizes on-line checkingi.
Accompanying drawing explanation
Fig. 1 is the full ion scan chromatogram of compound after makings is analyzed adopting purge and trap technology extraction sour flour dough steamed bun Hn to obtain in embodiment 1;
Fig. 2 is the full ion scan chromatogram of compound after makings is analyzed adopting purge and trap technology extraction sour flour dough steamed bun Sx to obtain in embodiment 1;
Fig. 3 is the full ion scan chromatogram of compound after makings is analyzed adopting purge and trap technology extraction sour flour dough steamed bun Gs to obtain in embodiment 1;
Fig. 4 is the full ion scan chromatogram of compound after makings is analyzed adopting purge and trap technology extraction sour flour dough steamed bun Hf to obtain in embodiment 1;
Fig. 5 is the full ion scan chromatogram of compound after makings is analyzed adopting purge and trap technology extraction sour flour dough steamed bun Hr to obtain in embodiment 1.
Embodiment
The present embodiment premised on technical solution of the present invention under implement, give detailed embodiment and process.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition.
Embodiment 1
1, sour flour dough: get five from the traditional zymotic sour flour dough of China different regions, be numbered Hn-87, Sx-91, Gs-107, Hf-112 and Hr-122.
2, to five sour flour doughs, respectively by following steps, prepare corresponding sour flour dough steamed bun, numbering is respectively Hn, Sx, Gs, Hf and Hr:
(1) sour flour dough is added to the water immersion, adds wheat flour after having soaked, mixing, is placed in temperature 30 DEG C, relative humidity 70% condition bottom fermentation 3.5h;
(2) after having fermented, add wheat flour and water, then carry out kneading dough, split, rub circle, shaping with the hands, then proof 60min under being placed in temperature 30 DEG C, relative humidity 75% condition;
(3) after having proofed, steam, obtain sour flour dough steamed bun.
3, respectively volatile flavor substance detection is carried out to five regional sour flour dough steamed bun samples as follows:
Get 100g sour flour dough steamed bun, after cooling 10min, stripping and slicing becomes particle diameter 80 object fritter, carries out purge and trap enrichment process, treatment conditions are: purging temperature is 40 DEG C, and purge flow rate is 25mL/min, and dry blowing temp is 20 DEG C, dryly blow time 2min, dry wind drift speed is 100mL/min;
Gas chromatography-mass spectrometry analysis technology is adopted to identify its volatile flavor substance after purging 50min, gas chromatography mass spectrometry instrument used is Agilent7890A-Agilent7000, adopt DB-WAX capillary chromatographic column (30m × 0.25mm × 0.25 μm), with Splitless injecting samples, carrier gas done by helium, flow rate of carrier gas is 1.0mL/min, and injector temperature is 240 DEG C;
Gas chromatography adopts temperature programme: initial temperature 40 DEG C, keeps 3min, is warming up to 200 DEG C, then is warming up to 230 DEG C with 10 DEG C/min with 5 DEG C/min, keeps 3min;
Mass spectrophotometry condition is: ionization mode is EI, ionization voltage 70eV, filament emission current 35 μ A, ion source temperature 230 DEG C, and interface temperature 280 DEG C, detection mode is full ion scan.
4, compound identification methods
GC-MS collection of illustrative plates, by computing machine and manual retrieval, contrasts authenticating compound each peak with the standard mass spectrogram that NIST Library08 provides, and the qualification result being only all greater than 700 when positive and negative matching degree is just listed; Being calculated the RI value of unknown compound by serial n-alkane, and compare with the compound R I value reported in www.odour.org.uk, is consistent in ± 50 scopes.Compounds content can calculate percentage contents by areas of peak normalization method.
RI = 100 × n + 100 × ( t a - t n ) t n + 1 - t n
In formula: RI is the retention time (min) of sample a;
T afor the retention time (min) of sample a;
T nfor n-alkane C nretention time (min).
The aroma compound that test findings adopts Purge & trap technology to extract five regional sour flour dough steamed buns respectively to detect after makings analysis in Table 1() and Fig. 1-5.
From result: purge and trap technology can carry out the analysis of wherein volatile flavor substance under the prerequisite not destroying sample, there is more stable detectability to aroma compounds such as loss easy in sample or easy ethanol, hexanal and the 3-methyl-1-butanols occurring to be oxidized, truly can reflect the characteristic flavor on basis component that sample itself exists.For the formation influence research of microbial metabolism in sour flour dough to steamed bun characteristic flavor on basis provides effective detection means.
Table 1Purge & trap combines the sour flour dough steamed bun flavor compound of GC/MS technology for detection

Claims (5)

1. the purge and trap detection method of volatile flavor substance in sour flour dough steamed bun, comprising:
(1) by after the cooling of sour flour dough steamed bun, stripping and slicing, scavenging trap is adopted to collect volatile flavor substance;
(2) gas chromatography-mass spectrometry analysis technology is adopted to identify described volatile flavor substance;
In step (1), the treatment conditions of described scavenging trap: purging temperature is 40-45 DEG C, purge time is 50-60min, purge flow rate is 25-30mL/min, dry blowing temp is 20-25 DEG C, dryly blows time 2-3min, and dry wind drift speed is 100-110mL/min;
In step (2), during gas chromatographic analysis, adopt following temperature programme: initial temperature 40 DEG C, keep 3min, be warming up to 200 DEG C with 5 DEG C/min, then be warming up to 230 DEG C with 10 DEG C/min, keep 3min;
In step (2), mass spectrophotometry condition is: ionization mode is EI, ionization voltage 70eV, filament emission current 35 μ A, ion source temperature 230 DEG C, and interface temperature 280 DEG C, detection mode is full ion scan.
2. purge and trap detection method according to claim 1, is characterized in that, in step (1), after described sour flour dough steamed bun stripping and slicing, particle diameter is 50-100 order.
3. purge and trap detection method according to claim 1, is characterized in that, the treatment conditions of described scavenging trap: purging temperature is 40 DEG C, purge time is 50min, and purge flow rate is 25mL/min, and dry blowing temp is 20 DEG C, dryly blow time 2min, dry wind drift speed is 100mL/min.
4. purge and trap detection method according to claim 1, is characterized in that, described sour flour dough steamed bun is prepared by the following method:
(1) sour flour dough is added to the water immersion, adds wheat flour after having soaked, mixing, is placed in temperature 28-32 DEG C, relative humidity 70-80% condition bottom fermentation 2.5-4h;
(2) after having fermented, add wheat flour and water, then carry out kneading dough, split, rub circle, shaping with the hands, then be placed in temperature 28-32 DEG C, proof 40-70min under relative humidity 70-80% condition;
(3) after having proofed, steam, obtain sour flour dough steamed bun.
5. purge and trap detection method according to claim 4, is characterized in that, in step (1), in every kilogram of sour flour dough, described immersion water consumption is 0.3-0.5kg, and the addition of wheat flour is 0.6-0.9kg; In step (2), in every kilogram of sour flour dough, the addition of described wheat flour is 1.1-1.4kg, and the addition of water is 0.5-0.8kg.
CN201310613183.XA 2013-11-26 2013-11-26 Purge-and-trap detection method of volatile flavor substances in sour-dough steamed bun Expired - Fee Related CN103675126B (en)

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CN111624290A (en) * 2020-05-11 2020-09-04 中国包装科研测试中心 Method for determining VOCs in packaging material by purging and trapping-gas chromatography-mass spectrometry

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