CN105092737A - Method for measuring types of volatile flavor compounds in steamed bun - Google Patents
Method for measuring types of volatile flavor compounds in steamed bun Download PDFInfo
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- CN105092737A CN105092737A CN201510540989.XA CN201510540989A CN105092737A CN 105092737 A CN105092737 A CN 105092737A CN 201510540989 A CN201510540989 A CN 201510540989A CN 105092737 A CN105092737 A CN 105092737A
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Abstract
The invention discloses a method for measuring the types of the volatile flavor compounds in a steamed bun. The method comprises the steps of after steaming, cooling and dicing the steamed bun, respectively placing into constant temperature metal baths of 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C and 100 DEG C to carry out pre-equilibration; adsorbing and extracting the volatile flavor compounds in the steamed bun subjected to pre-equilibration by adopting a headspace solid-phase microextraction technology; indentifying the volatile flavor compounds by utilizing a gas chromatography-mass spectrometry technology to obtain the types of the volatile flavor compounds in the steamed bun. According to the method provided by the invention, the headspace solid-phase microextraction technology and the gas chromatography-mass spectrometry technology are combined, different pre-equilibration temperatures are arranged, and specific extraction material and process are used, so that the volatile flavor compounds in the steamed bun can be comprehensively, quickly, and accurately detected, the operation is simple and the reliability of the result is high.
Description
Technical field
The present invention relates to flavour of food products technical field of chemistry, particularly relate to a kind of method measuring volatile flavor substance kind in steamed bun.
Background technology
Steamed bun is traditional staple food of China's especially northern area, originate from the period of Three Kingdoms according to legend, pass on from one to another as Zhuge Liang is invented, had the history of more than 1700 year, in the dietary structure of China, occupy critical role, the flour consumption made in order to steamed bun accounts for 40% of China's flour aggregate consumption.
Even to this day, people no longer content just to fill the stomach, and more focus on the characteristics such as the taste of food, local flavor.The method evaluating flavour of food products mainly comprises naked eyes evaluation and Instrument measuring two kinds of modes, although wherein naked eyes evaluation method more can reflect the flavor characteristics of food itself, but be often subject to the impact of personal like, the naked eyes evaluation result difference of different people is comparatively large, and can not quantitative measurement.
At present, the most frequently used local flavor assay method is chromatography of gases and mass spectrometric hyphenated technique, relies on separation function and comparatively perfect mass spectrum picture library that gas chromatography is powerful, can effectively carry out qualitative and quantitative analysis to the flavor substance of food.Flavor substance in food is carried out to the prerequisite that the pre-treatments such as separation and extraction are instrumental analysis, the method of now relatively more conventional food flavor substances separation and extraction has solvent extraction, distillation and extraction method, supercritical fluid extraction, head space method of trapping and direct thermal desorption method etc., wherein belong to the headspace solid-phase microextraction (solidphasemicro-extraction of head space method of trapping, SPME) technology directly can collect volatilization and nonvolatile compound from liquid or gaseous sample, can directly at GC, GC/MS and HPLC analyzes, it is a kind of centralized procurement sample, extraction, concentrated, sample introduction is in the new technology of one, it does not need solvent in local flavor leaching process, the pollution that can effectively avoid solvent extraction to bring, in flavour of food products analysis, there are bright prospects.
The application for a patent for invention of publication number CN103105440A discloses a kind of method measuring volatile flavor substance in bolete, and method is as follows: (1) adopts headspace solid-phase microextraction (HS-SPME) method to extract the volatile ingredient in bolete; (2) Gas chromatographyMass spectrometry is utilized to carry out separation qualification in conjunction with Kovats retention index (KI) to the volatile ingredient be extracted into; (3) gas chromatography-olfactometry (GC-0) is utilized to identify the volatile flavor substance in bolete.The method can analyze the volatile flavor component in bolete quickly and easily.
This technology also has certain application in the analysis of steamed bun local flavor, this patent is in harness basis, patent (patent No.: the ZL201310610998.2) content of application before us is carried out to the optimization of solid-phase microextraction condition, volatile flavor substance kind in steamed bun can be measured comprehensively, quickly and accurately.
Summary of the invention
The invention provides a kind of method measuring volatile flavor substance in steamed bun, the method can measure the volatile flavor substance in steamed bun more comprehensively, quickly and accurately.
Measure a method for volatile flavor substance kind in steamed bun, comprising:
(1) will cook, cool, after stripping and slicing, being placed in temperature will respectively be that the constant-temperature metal bath of 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C and 100 DEG C carries out pre-equilibration;
(2) headspace solid-phase microextraction technology is adopted to carry out sorption extraction to the volatile flavor substance in the steamed bun after five groups of pre-equilibrations;
(3) utilize gas chromatography-mass spectrometry analysis technology to identify volatile flavor substance, obtain the kind of volatile flavor substance in steamed bun.
Adopt headspace solid-phase microextraction technology can effective separating volatile components, recycle mass spectrogram analysis and retention index methods combining, can accurately differentiate volatile compound to be measured.
Pre-equilibration temperature is the extraction temperature of subsequent sample, and the object of pre-equilibration is to make sample be stable at the extraction temperature of needs, makes the volatile flavor substance in sample evaporate in sample bottle simultaneously, is conducive to the follow-up extraction process of sample.
In step (1), the cool time of described steamed bun is 4 ~ 6 minutes, is convenient to steamed bun stripping and slicing.
After described steamed bun stripping and slicing, be 0.2 ~ 0.4cm
3blockage, be beneficial to extraction.By described pre-equilibration, steamed bun flavor substances can be made fully to evaporate, form the concentration of relative saturation at sample bottle head space, effectively can improve effect of extracting.
As preferably, in step (1), the time of pre-equilibration is 10 ~ 20min; More preferably, the time is 15min.
In step (2), described headspace solid-phase microextraction adopts 75 μm of Carboxen/PDMS extracting head (carbonaceous molecular sieve/dimethyl silicone polymer), compared with other extracting head, the extracting head that the present invention adopts has stronger adsorptive power to volatile flavor substance in sample, and effect of extracting is more stable.
In step (2), during headspace solid-phase microextraction, the extraction temperature often organizing steamed bun is identical with pre-equilibration temperature in step (1), that is: the pre-equilibration temperature often organized and extraction temperature are corresponding one by one, and extraction time is 30 ~ 90min; More preferably, the time is 60min.
In step (2), after extraction terminates, carry out desorption parsing, the temperature that desorption is resolved is 250 DEG C, and the time is 1 ~ 8min; As preferably, the time that desorption is resolved is 5min.
In step (3), 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 220 DEG C with 10 DEG C/min, keep 3min.Find that this heating schedule is best to the separating effect of volatile flavor substance in sample by test, reproducible.
In step (3), during gas chromatographic analysis, the chromatographic column model of employing is DB-WAX (30m × 0.25mm × 0.25 μm).
In step (3), mass spectrophotometry condition is: electron energy is 70eV, ion source temperature 230 DEG C, and level Four bar temperature is 150 DEG C, and detection mode is full ion scan, sweep limit 10-500m/z; Preferred sweep limit is 35-495m/z.
In step (3), the mass spectrogram of acquisition and NIST11 standard substance database are compared, positive and negative matching degree is all more than or equal to 800.In NIST retrieval, matching rate is 1000 to the maximum, and best result is 999, and the spectrogram without peak is 0.Generally, 900 or higher, excellent match; 800-900, matched well; 700-800, Shang Ke; Lower than 600, poor.Generally, wanting credible result matching degree should higher than 800, and therefore, the standard of the material that we choose is that matching degree is more than or equal to 800.
Compared with prior art, the present invention has following beneficial effect:
Headspace solid-phase microextraction technology and gas chromatography-mass spectrometry analysis technology combine by the inventive method, and different pre-equilibration temperature is set, volatile flavor substance in steamed bun is detected more comprehensively, quickly and accurately, and simple to operate, the Feasible degree of result is high.
Accompanying drawing explanation
Fig. 1 adopts different extracting head to the comparison (60 DEG C) of the adsorptive power of volatile matter in steamed bun;
A：100μmPDMS；B：65μmPDMS/DVB；C：50/30μmDVB/CAR/PDMS；D：75μmCarboxen/PDMS。
Fig. 2 is different extracting head comparing the absorption of volatile matter in steamed bun and identification capacity.
Fig. 3 is the comparison of volatile species in steamed bun under different extraction time.
Fig. 4 is the comparison detecting volatile flavor substance in steamed bun under different desorption time.
Embodiment
Below in conjunction with specific embodiments and the drawings, the present invention is described in further detail.
Embodiment 1
Measure a method for volatile flavor substance kind in steamed bun, comprise the following steps:
(1), after just steamed steamed bun being cooled 5 minutes, 0.3cm is cut into
3fritter, take 3.0g and be placed in the headspace analysis sample bottle that volume is 20mL;
(2) get the sample bottle 5 prepared in step (1), the constant-temperature metal bath being placed in 60,70,80,90,100 DEG C respectively balances 15 minutes;
(3) after balance terminates, extracting head is inserted in sample bottle, at corresponding temperature (60,70,80,90,100 DEG C), extract 60 minutes respectively, the model of extracting head is 75 μm of Carboxen/PDMS (carbonaceous molecular sieve/dimethyl silicone polymers);
(4), after extraction terminates, extracting head is inserted gas chromatographic sample introduction mouth and carry out desorption parsing, the temperature of injection port is 250 DEG C, and desorption time is 5 minutes;
(5) flavor substance of Gas chromatographyMass spectrometry to absorption is utilized to identify, chromatographic column model is DB-WAX (30m × 0.25mm × 0.25 μm), carrier gas is high-purity helium (99.999%), and flow velocity is 1ml/min.Heating schedule is: initial temperature 40 DEG C, keeps 3min, is warming up to 200 DEG C, then is warming up to 220 DEG C with 10 DEG C/min with 5 DEG C/min, keeps 3min; Mass Spectrometry Conditions is: electron energy is 70eV, ion source temperature 230 DEG C, and level Four bar temperature is 150 DEG C, and detection mode is full ion scan, sweep limit 30-500m/z.
(6) mass spectrogram of acquisition and NIST11 standard substance database are compared, positive and negative matching degree is all more than or equal to 800 and lists, and determines classes of compounds in conjunction with RI value etc., and result is as follows.
The difference of volatile flavor substance kind in steamed bun under the different equilibrium temperature of table 1 and extraction temperature
Comparative example 1
This comparative example is except extracting head is different from embodiment 1, and all the other steps are all identical; The extracting head adopted is 100 μm of PDMS, and result as shown in Figure 1 and Figure 2.
Comparative example 2
This comparative example is except extracting head is different from embodiment 1, and all the other steps are all identical; The extracting head adopted is 65 μm of PDMS/DVB, and result as shown in Figure 1 and Figure 2.
Comparative example 3
This comparative example is except extracting head is different from embodiment 1, and all the other steps are all identical; The extracting head adopted is 50/30 μm of DVB/CAR/PDMS, and result as shown in Figure 1 and Figure 2.
Embodiment 2
Except setting different extraction time in the present embodiment, be respectively: 30min, 60min, 90min, 120min, all the other steps are all identical; Result as shown in Figure 3.
Embodiment 3
Except setting different desorption time in the present embodiment, be respectively: 1min, 2min, 3min, 4min, 5min, 6min; All the other steps are all identical; Result as shown in Figure 4.
Claims (8)
1. measure a method for volatile flavor substance kind in steamed bun, it is characterized in that, comprising:
(1) steamed bun cooked, cool, after stripping and slicing, being placed in temperature is respectively that the constant-temperature metal bath of 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C and 100 DEG C carries out pre-equilibration;
(2) headspace solid-phase microextraction technology is adopted to carry out sorption extraction to the volatile flavor substance in the steamed bun after five groups of pre-equilibrations;
(3) utilize gas chromatography-mass spectrometry analysis technology to identify volatile flavor substance, obtain the kind of volatile flavor substance in steamed bun.
2. the method for claim 1, is characterized in that, in step (1), the time of pre-equilibration is 10 ~ 20min.
3. the method for claim 1, is characterized in that, in step (2), described headspace solid-phase microextraction adopts 75 μm of Carboxen/PDMS extracting head.
4. the method for claim 1, is characterized in that, in step (2), during headspace solid-phase microextraction, the extraction temperature often organizing steamed bun is identical with pre-equilibration temperature in step (1), and extraction time is 30 ~ 90min.
5. the method for claim 1, is characterized in that, in step (2), after extraction terminates, carry out desorption parsing, the temperature that desorption is resolved is 250 DEG C, and the time is 1 ~ 8 minute.
6. the method for claim 1, is characterized in that, in step (3), 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 220 DEG C with 10 DEG C/min, keep 3min.
7. the method for claim 1, is characterized in that, in step (3), during gas chromatographic analysis, the chromatographic column model of employing is DB-WAX (30m × 0.25mm × 0.25 μm).
8. the method for claim 1, is characterized in that, in step (3), mass spectrophotometry condition is: electron energy is 70eV, ion source temperature 230 DEG C, and level Four bar temperature is 150 DEG C, and detection mode is full ion scan, sweep limit 10-500m/z.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107179375A (en) * | 2017-07-06 | 2017-09-19 | 浙江大学 | A kind of method of volatile flavor substance in ultrasonic method auxiliary measuring brown rice |
| TWI729717B (en) * | 2020-03-02 | 2021-06-01 | 統一企業股份有限公司 | Analyzing method for aroma of dough and system of the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675124A (en) * | 2013-11-26 | 2014-03-26 | 浙江大学 | Headspace solid phase microextraction detection method for volatile flavor substances in sour dough steamed buns |
| CN103675126A (en) * | 2013-11-26 | 2014-03-26 | 浙江大学 | Purge-and-trap detection method of volatile flavor substances in sour-dough steamed bun |
-
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- 2015-08-28 CN CN201510540989.XA patent/CN105092737A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675124A (en) * | 2013-11-26 | 2014-03-26 | 浙江大学 | Headspace solid phase microextraction detection method for volatile flavor substances in sour dough steamed buns |
| CN103675126A (en) * | 2013-11-26 | 2014-03-26 | 浙江大学 | Purge-and-trap detection method of volatile flavor substances in sour-dough steamed bun |
Non-Patent Citations (4)
| Title |
|---|
| YANGSOO KIM 等: "Spontaneous sourdough processing of Chinese Northern-style steamed breads and their volatile compounds", 《FOOD CHEMISTRY》 * |
| YUYU ZHANG 等: "Preparation and Aroma Analysis of Chinese Traditional Fermented Flour Paste", 《FOOD SCI. BIOTECHNOL.》 * |
| 苏东海 等: "固相微萃取分析传统老酵头馒头挥发性物质", 《食品研究与开发》 * |
| 顾沁 等: "小麦蛋白酶水解制备面包风味前体物质的研究", 《食品与生物技术学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107179375A (en) * | 2017-07-06 | 2017-09-19 | 浙江大学 | A kind of method of volatile flavor substance in ultrasonic method auxiliary measuring brown rice |
| CN107179375B (en) * | 2017-07-06 | 2020-02-21 | 浙江大学 | Method for measuring volatile flavor substances in brown rice with assistance of ultrasonic method |
| TWI729717B (en) * | 2020-03-02 | 2021-06-01 | 統一企業股份有限公司 | Analyzing method for aroma of dough and system of the same |
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