CN102944624A - Method for detecting sulfocompound in volatile flavor substances of fermented meat product - Google Patents
Method for detecting sulfocompound in volatile flavor substances of fermented meat product Download PDFInfo
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- CN102944624A CN102944624A CN2012104762541A CN201210476254A CN102944624A CN 102944624 A CN102944624 A CN 102944624A CN 2012104762541 A CN2012104762541 A CN 2012104762541A CN 201210476254 A CN201210476254 A CN 201210476254A CN 102944624 A CN102944624 A CN 102944624A
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Abstract
The invention discloses a method for detecting a sulfocompound in volatile flavor substances of a fermented meat product. The method includes the following steps of firstly, slicing the fermented meat product into slices with thickness smaller than 0.5mm, rapidly spreading the slices at a dried conical flask bottom, sealing a conical flask opening with silver paper and then sealing the conical flask opening with a sealing film; secondly, using an extraction fiber and a manual injector, subjecting the extraction fiber to ageing at an injection port of a gas chromatograph at the temperature of 250 DEG C for 2 hours, placing a conical flask containing the fermented meat product slices in the first step in a water bath kettle with the temperature of 60 DEG C to be balanced for 10 minutes, and inserting the aged extraction fiber into the conical flask opening for extraction for 40 minutes; thirdly, inserting the aged and extracted extraction fiber in the injection port of the gas chromatograph for desorption at the temperature of 250 DEG C for 2 minutes, and then using gas chromatography-flame photometric detectors to collect data; and fourthly, subjecting the data which are collected in the third step to statistics and data analysis. The method is advanced and simple, and the gas chromatography-flame photometric detectors are combined so that accuracy of detection results is greatly improved.
Description
Technical field
The present invention relates to sulfocompound detection method in a kind of fermentation meat product volatile flavor substance is to utilize gas chromatography-flame photometric detector (FPD) to detect the method for volatile flavor substance in the food, press International Patent Classification (IPC) (IPC) and divide, belong in physics-instrument branch by means of the chemistry of measuring material physical property is tested or analysis of material (G01N) in need utilize the suction-operated classification.
Background technology
Sulfocompound is mainly generated by sulfur-containing amino acid in the fermentation meat product volatile flavor substance, produces mercaptan (thiols) such as methionine etc. through the Strecker degraded, and further oxidation forms sulfocompound.Volatile sulfur compound becomes the significant contribution factor of flavor of fermented meat products because having lower taste threshold.Volatile sulfur compound does not have independent detection method in the fermentation meat product at present, generally measures with all volatile matter with the method for gas chromatography-mass spectrography technology, while distillation extraction or Electronic Nose by the headspace solid-phase microextraction technology.But because volatile sulfur compound content is lower, may extract less than such material with distillation extraction technology simultaneously, and need with an organic solvent repeatedly extraction during extraction, operator's health is had certain influence, discarded object also pollutes environment.And with gas chromatography combined with mass spectrometry technology or Electronic Nose can be because of detection material too many and other material abundance can not go out the peak greatly, so be easy to undetected.In addition, the pre-treating method that detects at present mostly employing is cut into broken end or processes with liquid nitrogen.Being easy to like this generation owing to water vapor in heating process forms fine and close meatball volatile matter can not be evaporated, therefore the volatile sulfur compound of trace more is difficult for being detected, affect the correctness of testing result, thereby impact is to the correct judgement of meat products local flavor.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists for above-mentioned prior art, and sulfocompound detection method in a kind of fermentation meat product volatile flavor substance is provided.The technical matters that solves has, and at first, in the pre-treatment link, fermentation meat product is thinly sliced, and the minced meat that can avoid commonly using forms afterwards fine and close " meat pie " and hinders the volatile matter effusion in heating.Secondly, changing gas chromatography-mass spectrography is gas chromatography-flame photometric detector (FPD) coupling.Flame photometric detector (FPD) is the specific detectors that is used for specially detecting sulfocompound.Although the sulfocompound taste threshold is low, relative content is also very low.So can avoid with specific detectors that affecting it goes out the peak greatly because of other volatile matter abundance, cause undetected.
Technical scheme of the present invention is, sulfocompound detection method in the fermentation meat product volatile flavor substance, it is characterized in that, fermentation meat product is cut into slices, adopt headspace solid-phase microextraction and gas chromatography-flame photometric detector (FPD) coupling, volatile sulfur compounds in the fermentation meat product is carried out qualitative and quantitative analysis, may further comprise the steps:
1) fermentation meat product pre-treatment, with the fermentation meat product section, slice thickness is tiled in rapidly at the bottom of the dry conical flask less than the thin slice of 0.5mm, and bottleneck with the tinfoil sealing, then seals with sealed membrane first;
2) extraction is adopted extracting head, manual injector, extracting head first at gas chromatograph injection port in 250 ℃ of aging 2 h, the conical flask that step 1) is equipped with the fermentation meat product section is put in 60 ℃ water-bath balance 10 min, and the extracting head that then will wear out is inserted bottleneck, extraction 40min;
3) sample introduction is with step 2) aging extraction extracting head insertion gas chromatograph injection port well, in 250 ℃ of lower desorb 2 min, then begin with gas chromatography-flame photometric detector (FPD) image data;
4) to the step 3) image data add up, data analysis.
Step 2) described extracting head is combined type 75 um Car/PDMS extracting head, and described manual injector is manual SPME injector.
The inventive method is advanced simple, and main testing process is as follows: cut into slices → divide in container bottom → extraction → sample introduction → detection → statistics.Mainly by increasing fermentation meat product and air contact area, the method that reduces other material absorption improves the abundance that detects of sulfocompound with gas chromatography-flame photometric detector (FPD).Can fast detecting and the accurate quantitative analysis fermentation meat product in volatile sulfur compounds, quantitative limit can be low to moderate 0.02 μ g/L, linear dependence coefficients R
2All greater than 0.98, relative standard deviation is less than 20%.The headspace solid-phase microextraction technology need not organic solvent, avoids the active sulfide of some chemical property to decompose, effectively the sulfide in the enrichment fermentation meat product; The single-minded detection sulfide of flame photometric detector (FPD) has been got rid of the interference of other material, has greatly improved result's accuracy.Simultaneously in testing process, avoid with an organic solvent waiting chemical reagent, not only reduce the harm to operator's health, also reduce causing harm to environment.With headspace solid-phase microextraction and gas chromatography-flame photometric detector (FPD) coupling technique the volatile sulfur compounds in the fermentation meat product is carried out qualitative and quantitative analysis, have great significance to improving the fermentation meat product quality.
Headspace solid-phase microextraction-gas chromatography-flame photometric detector (FPD) coupling technique is simple to operate, and required time is short, favorable reproducibility.Be fit to general scientific research institutions, colleges and universities and relevant enterprise and carry out the flavor of fermented meat products detection.But headspace solid-phase microextraction equipment Reusability.Therefore, only need there be a gas chromatography-flame photometric detector (FPD) just can advance detection in batches, and guarantees that the result's is reliable and stable.
Embodiment
Sulfocompound detection method in the fermentation meat product volatile flavor substance, fermentation meat product is cut into slices, with headspace solid-phase microextraction and gas chromatography-flame photometric detector (FPD) coupling technique, the volatile sulfur compounds in the fermentation meat product is carried out qualitative and quantitative analysis, concrete steps are as follows:
1, fermentation meat product pre-treatment
10 gram fermentation meat products are cut into thickness less than the thin slice of 0.5mm, are tiled in rapidly at the bottom of the dry conical flask, bottleneck with the tinfoil sealing, then seals with sealed membrane first.
2, extraction
Combined type 75 um Car/PDMS extracting head, manually SPME injector (SUPELCO, USA).Extracting head is used first at gas chromatograph injection port for the first time in 250 ℃ of aging 2 h.The conical flask that fermented meat is housed is put in 60 ℃ water-bath balance 10 min, and the extracting head that then will wear out is inserted bottleneck, extraction 40min.
3, sample introduction
Extracting head is inserted gas chromatograph injection port, in 250 ℃ of lower desorb 2 min, then begin with gas chromatography-flame photometric detector (FPD) image data.
Chromatographic column: OV1701 quartz capillary column (30m * 0.25 mm * 0.3 μ m), coating is: Poly (dimthyldiloxy) poly (Isosorbide-5-Nitrae-bis (dimethylsiloxy) phenylene) siloxane); Carrier gas is He, flow 0.8mL/min; Injector temperature is 250 ℃; Do not shunt; Temperature programme is: 32 ℃ keep 10min → 32 ℃ (3 ℃/min) → 160 ℃, 160 ℃ keep 5min.
4, data analysis.
Claims (4)
1. sulfocompound detection method in the fermentation meat product volatile flavor substance, it is characterized in that, fermentation meat product is cut into slices, adopt headspace solid-phase microextraction and gas chromatography-flame photometric detector (FPD) coupling, volatile sulfur compounds in the fermentation meat product is carried out qualitative and quantitative analysis, may further comprise the steps:
1) fermentation meat product pre-treatment is cut into thickness less than the thin slice of 0.5mm with fermentation meat product, is tiled in rapidly at the bottom of the dry conical flask, and bottleneck with the tinfoil sealing, then seals with sealed membrane first;
2) extraction is adopted extracting head, injector, extracting head first at gas chromatograph injection port in 250 ℃ of aging 2 h, the conical flask that step 1) is equipped with the fermentation meat product thin slice is put in 60 ℃ water-bath balance 10 min, and the extracting head that then will wear out is inserted bottleneck, extraction 40min;
3) sample introduction is with step 2) aging extraction extracting head insertion gas chromatograph injection port well, in 250 ℃ of lower desorb 2 min, then begin with gas chromatography-flame photometric detector (FPD) image data;
4) to the step 3) image data add up, data analysis.
2. sulfocompound detection method in the fermentation meat product volatile flavor substance according to claim 1 is characterized in that step 2) described extracting head is combined type 75 um Car/PDMS extracting head.
3. sulfocompound detection method in the fermentation meat product volatile flavor substance according to claim 1 is characterized in that step 2) described injector is manual SPME injector.
4. sulfocompound detection method in the fermentation meat product volatile flavor substance according to claim 1 is characterized in that, the described detecting device of step 3) is flame photometric detector (FPD).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823836A (en) * | 2016-03-11 | 2016-08-03 | 中国农业科学院农产品加工研究所 | Sauce braised meat product flavor active substance profile analysis method |
| CN111323505A (en) * | 2020-03-18 | 2020-06-23 | 中国农业科学院兰州畜牧与兽药研究所 | Method for detecting sulfur-containing compounds in volatile flavor substances of fermented meat products |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020024672A1 (en) * | 2000-07-11 | 2002-02-28 | Shimadzu Corporation | Flame photometric detector |
| US7291478B1 (en) * | 2005-03-29 | 2007-11-06 | The United States Of America As Represented By The Secretary Of The Army | Rapid screening and analysis of present and potential nerve agents and their degradation products |
| CN101393178A (en) * | 2008-10-30 | 2009-03-25 | 中国农业科学院北京畜牧兽医研究所 | Fermentation beef ham identification method |
-
2012
- 2012-11-22 CN CN2012104762541A patent/CN102944624A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020024672A1 (en) * | 2000-07-11 | 2002-02-28 | Shimadzu Corporation | Flame photometric detector |
| US7291478B1 (en) * | 2005-03-29 | 2007-11-06 | The United States Of America As Represented By The Secretary Of The Army | Rapid screening and analysis of present and potential nerve agents and their degradation products |
| CN101393178A (en) * | 2008-10-30 | 2009-03-25 | 中国农业科学院北京畜牧兽医研究所 | Fermentation beef ham identification method |
Non-Patent Citations (7)
| Title |
|---|
| DA-MI JUNG 等: "Headspace Solid-Phase Microextraction Method for the Study of the Volatility of Selected Flavor Compounds", 《J. AGRIC. FOOD CHEM》 * |
| FABIO PELUSIO 等: "Headspace Solid-Phase Microextraction Analysis of Volatile Organic Sulfur Compounds in Black and White Truffle Aroma", 《J. AGRIC. FOOD CHEM》 * |
| MATTHIAS GUNTERT 等: "Identification and Formation of Some Selected Sulfur-Containing Flavor Compounds in Various Meat Model Systems", 《J. AGRIC. FOOD CHEM》 * |
| 张春晖 等: "顶空固相微萃取-气相色谱-质谱分析发酵香肠挥发性成分", 《分析科学学报》 * |
| 杜喜玲: "气质色谱法测定发酵肉风味物质的研究", 《肉类工业》 * |
| 王家林 等: "啤酒中硫化物分析方法研究进展", 《酿酒科技》 * |
| 田怀香 等: "顶空固相微萃取-气相色谱-质谱法分离鉴定金华火腿的挥发性风味物质", 《色谱》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823836A (en) * | 2016-03-11 | 2016-08-03 | 中国农业科学院农产品加工研究所 | Sauce braised meat product flavor active substance profile analysis method |
| CN111323505A (en) * | 2020-03-18 | 2020-06-23 | 中国农业科学院兰州畜牧与兽药研究所 | Method for detecting sulfur-containing compounds in volatile flavor substances of fermented meat products |
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Application publication date: 20130227 |