CN106645495A - Detection method for volatile components of sugar - Google Patents
Detection method for volatile components of sugar Download PDFInfo
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- CN106645495A CN106645495A CN201611250323.1A CN201611250323A CN106645495A CN 106645495 A CN106645495 A CN 106645495A CN 201611250323 A CN201611250323 A CN 201611250323A CN 106645495 A CN106645495 A CN 106645495A
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- volatile components
- smelling
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- 238000001514 detection method Methods 0.000 title claims abstract description 49
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000010606 normalization Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 23
- 238000001179 sorption measurement Methods 0.000 claims description 16
- CZMRCDWAGMRECN-UHFFFAOYSA-N Rohrzucker Natural products OCC1OC(CO)(OC2OC(CO)C(O)C(O)C2O)C(O)C1O CZMRCDWAGMRECN-UHFFFAOYSA-N 0.000 claims description 14
- 239000012159 carrier gas Substances 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 10
- 238000004949 mass spectrometry Methods 0.000 claims description 9
- 238000004445 quantitative analysis Methods 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 8
- 238000004451 qualitative analysis Methods 0.000 claims description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 3
- 230000001953 sensory effect Effects 0.000 abstract description 14
- 238000011156 evaluation Methods 0.000 abstract description 9
- 239000012071 phase Substances 0.000 abstract description 4
- 238000001228 spectrum Methods 0.000 abstract description 3
- 238000007781 pre-processing Methods 0.000 abstract 2
- 210000003128 head Anatomy 0.000 description 26
- 238000012360 testing method Methods 0.000 description 11
- 239000000796 flavoring agent Substances 0.000 description 10
- 235000019634 flavors Nutrition 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 239000007790 solid phase Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000012797 qualification Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Natural products C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 3
- 241001062472 Stokellia anisodon Species 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 3
- 235000019580 granularity Nutrition 0.000 description 3
- 210000000697 sensory organ Anatomy 0.000 description 3
- 238000002470 solid-phase micro-extraction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 1
- LCZUOKDVTBMCMX-UHFFFAOYSA-N 2,5-Dimethylpyrazine Chemical class CC1=CN=C(C)C=N1 LCZUOKDVTBMCMX-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 1
- 150000000644 6-membered heterocyclic compounds Chemical group 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004853 microextraction Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 150000003216 pyrazines Chemical class 0.000 description 1
- 125000003373 pyrazinyl group Chemical group 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- -1 saccharide compound Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 235000019615 sensations Nutrition 0.000 description 1
- 230000008786 sensory perception of smell Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a detection method for volatile components of sugar. The detection method comprises the following steps: preprocessing the sugar, performing the headspace solid-phase micro-extraction on the preprocessed sugar, extracting volatile components, and detecting the volatile components by adopting a gas-phase chromatography-mass spectrometry-sniffing method; and qualitatively and quantitatively analyzing the volatile components by virtue of a spectrum library-area normalization method, and identifying smell intensity and type by virtue of sniffing. A sugar sample is directly processed by virtue of the headspace solid-phase micro-extraction, the volatile components are gathered, and no complicated preprocessing step is needed; and the volatile components are detected by using the gas-phase chromatography-mass spectrometry-sniffing method, and the smell type and intensity of the volatile components are synchronously identified while the volatile components are qualitatively and quantitatively identified, so that the method is simple, and the identification result is accurate. Compared with the sensory evaluation and compared with the prior art, the detection method is more approximate to the real sensory identification result. A reference is provided for tracing the source of the product.
Description
Technical field
The present invention relates to technical field of analytical chemistry, more particularly, to a kind of detection method of the volatile component of sugar.
Background technology
Used as two big sources of food sugar, beet sugar and cane suger occupy main status in daily life.
As product that is familiar and liking, although the Main Ingredients and Appearance of beet sugar and cane suger is all sucrose, due to raw material and process
The difference of technique, as some micro or even trace components both sugared local flavors can be have impact on, and cause different sense organ wind
Taste.It is domestic at present to be directed to the sugared local flavor composition analysis shorter mention of food.
Calendar year 2001, PerEt al. (PerMats Larsson,Anders Leufve′n,and
Hans Lingnert., J.Agric.Food Chem.2000,48:GC-MS analysis shows 4844-4850) are adopted, it is special with sense organ
Levying the main matter of correlation has a lot, wherein two class materials occupy main positions, one is Pyrazine, and two is short chain volatile fat
Acids (including acetic acid, propionic acid, butyric acid, isovaleric acid etc.).Pyrazine is 6-membered heterocyclic compound of the Isosorbide-5-Nitrae position containing two nitrogen-atoms,
With strong pyridine taste, soluble in water, ethanol, ether etc., can volatilize with vapor.If aminated compounds and also
The presence of former saccharide compound, under uniform temperature and ambient condition, it is possible to produce pyrazine compounds composition.
S.J.Moore et al. has also delivered the correlative study of the volatile component composition that have detected beet sugar, but article
The variation tendency of short chain organic acid is concerned only with, other components has been related to less.Marsili is to causing the chemical combination of beet sugar peculiar smell
The identification of thing and it is quantitative (Marsili, Journal of Chromatographic Science, 1994,32:165-171.) recognize
Fixed 2,5- dimethyl pyrazines are possible to cause one of compound of characteristic off flavor of beet sugar.In this document before odor trap
After process needs to dissolve solid sample with defoamer and water, sugar juice is purged using hot-air is added.Brought about the desired sensation
Taste needs the dewatered steam link through an extra addition to remove the impact of moisture content, ability in the desorption through 75min
It is analyzed into chromatographic column, operating process is complicated and takes.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of detection method of the volatile component of sugar,
The detection method that the present invention is provided is simple, and qualification result is accurate, closer in actual naked eyes evaluation result.
The invention provides a kind of detection method of the volatile component of sugar, including：
Jing headspace solid-phase microextractions extract volatile ingredient after sugar pretreatment, are carried out using gas chromatography-mass spectrum-smelling method
Detection；
The adsorption temp of the extracting head of the headspace solid-phase microextraction is 70～120 DEG C；Adsorption time is 5～60min；
The detection parameter of the gas chromatography-mass spectrum-smelling is as follows：
Chromatographic condition：Chromatographic column is HP-5 capillary chromatographic columns；1～1.2mL/min of flow rate of carrier gas；
Temperature programming is：50～55 DEG C of initial temperature, keeps 1～3min；100 are warming up to the speed of 5～6 DEG C/min～
110℃；220～240 DEG C are warmed up to the speed of 10～11 DEG C/min, 5～8min is kept；
Mass Spectrometry Conditions：Ion gun:EI sources；Electron energy 70ev；230～240 DEG C of ion source temperature；
Smelling condition：200～210 DEG C of interface temperature；
Qualitative and quantitative analysis is carried out to volatile component by composing storehouse and area normalization method, it is strong to smell by smelling
Degree and type are identified.
Preferably, the adsorption temp of the extracting head of the headspace solid-phase microextraction is 80～120 DEG C；Adsorption time be 15～
45min。
Preferably, the extracting head of the headspace solid-phase microextraction is extracting fiber, and the extracting fiber is DVB/CAR/
PDMS；Carrier thickness is 30～50 μm.
Preferably, the sugared mixing speed of the headspace solid-phase microextraction is 200～300rpm/min.
Preferably, the desorption temperature of the extracting head of the headspace solid-phase microextraction is 240～250 DEG C；The desorption time
For 2～5min.
Preferably, the chromatographic condition is specially：
HP-5 capillary chromatographic columns, 30m*0.25mm*0.25 μm；Carrier gas：He；1～1.2mL/min of flow rate of carrier gas；Sample introduction
Mouth temperature is 240～250 DEG C；Split sampling, split ratio is 1:1；
Temperature programming is：50～53 DEG C of initial temperature, keeps 1～2min；100 are warming up to the speed of 5～5.5 DEG C/min
～110 DEG C；220～230 DEG C are warmed up to the speed of 10 DEG C/min, 5～8min is kept.
Preferably, the Mass Spectrometry Conditions are specially：
Ion gun:EI sources；Electron energy 70ev；250～260 DEG C of transmission line temperature；230～240 DEG C of ion source temperature；Four
Level bar temperature is 150 DEG C；Solvent delay 1min；Sweep limits 55～500.
Preferably, the interface temperature of the smelling is 200 DEG C.
Preferably, the sugar is including one or more in beet sugar and cane suger.
Preferably, to crush, the granularity of crushing is less than 0.2mm for the pretreatment of the sugar.
Compared with prior art, the invention provides it is a kind of sugar volatile component detection method, including：Sugar pretreatment
Volatile ingredient is extracted by headspace solid-phase microextraction, is detected using gas chromatography-mass spectrum-smelling method；The head space is consolidated
The adsorption temp of the extracting head of phase extraction is 70～120 DEG C；Adsorption time is 5～60min；The gas chromatography-mass spectrum-smell
The detection parameter of news is as follows：Chromatographic condition：Chromatographic column is HP-5 capillary chromatographic columns；1～1.2mL/min of flow rate of carrier gas；Program
Heat up and be：50～55 DEG C of initial temperature, keeps 1～3min；100～110 DEG C are warming up to the speed of 5～6 DEG C/min；With 10～
The speed of 11 DEG C/min is warmed up to 220～240 DEG C, keeps 5～8min；Mass Spectrometry Conditions：Ion gun:EI sources；Electron energy 70ev；
230～240 DEG C of ion source temperature；Smelling condition：200～210 DEG C of interface temperature；By composing storehouse and area normalization method to volatilization
Property component carries out qualitative and quantitative analysis, and odour intensity and type are identified by smelling.The present invention passes through head space solid phase
Micro-extraction is directly processed sugar-like product, concentrating volatile component, without the need for complicated pre-treatment step；Gas phase color is utilized simultaneously
Spectrum-mass spectrum-smelling method detects to volatile component, while qualitative and Quantitative measurement is carried out to volatile component for
The odor types and intensity of volatile component have carried out synchronous identification, and method is simple, and qualification result is accurate.And with subjective appreciation
Compare, hinge structure, closer in closer in actual naked eyes evaluation result.Carry out tracing to the source providing for product is specific
With reference to.Have ten simultaneously for the difference analysis of the different product smell quality sugared for actual production and application and raising
Divide important meaning.
Description of the drawings
Fig. 1 is the GC-MS figures of the detection of the embodiment of the present invention 1；
The GC-MS figures that Fig. 2 embodiment of the present invention 2 is surveyed；
The GC-MS figures of Fig. 3 inventive embodiments 3；
The GC-MS figures of Fig. 4 inventions comparative example 1.
Specific embodiment
The invention provides a kind of detection method of the volatile component of sugar, including：
Jing headspace solid-phase microextractions extract volatile ingredient after sugar pretreatment, are carried out using gas chromatography-mass spectrum-smelling method
Detection；
The adsorption temp of the extracting head of the headspace solid-phase microextraction is 70～120 DEG C；Adsorption time is 5～60min；
The detection parameter of the gas chromatography-mass spectrum-smelling is as follows：
Chromatographic condition：Chromatographic column is HP-5 capillary chromatographic columns；1～1.2mL/min of flow rate of carrier gas；
Temperature programming is：50～55 DEG C of initial temperature, keeps 1～3min；100 are warming up to the speed of 5～6 DEG C/min～
110℃；220～240 DEG C are warmed up to the speed of 10～11 DEG C/min, 5～8min is kept；
Mass Spectrometry Conditions：Ion gun:EI sources；Electron energy 70ev；230～240 DEG C of ion source temperature；
Smelling condition：200～210 DEG C of interface temperature；
Qualitative and quantitative analysis is carried out to volatile component by composing storehouse and area normalization method, it is strong to smell by smelling
Degree and type are identified.
The present invention is first by sugar pretreatment.
Sugar of the present invention is preferably one or more in beet sugar and cane suger.The pretreatment of the sugar is preferably concrete
It is that Icing Sugar is broken, the present invention is not defined for the concrete mode crushed, preferably pulverizer is crushed.Preferably sieve after crushing
Point, the sieve is preferably round-hole mesh, and screening obtains the particle of following granularities.The granularity is preferably less than 0.2mm；More preferably
Less than 0.15mm.
After crushing, mix, load and sealed after container, it is stand-by.
After crushing, Jing headspace solid-phase microextractions extract volatile ingredient.
The present invention is not defined for the headspace solid-phase microextraction instrument, head space solid phase well known to those skilled in the art
Micro-extraction instrument.
In the present invention, the extracting head of the headspace solid-phase microextraction is preferably extracting fiber, and the extracting fiber is
DVB/CAR/PDMS；Carrier thickness is preferably 30～50 μm.
In the present invention, the adsorption temp of the extracting head of the headspace solid-phase microextraction is 70～120 DEG C；Preferably 80～
120℃；More preferably 90～110 DEG C；Adsorption time is 5～60min；Preferably 15～45min；More preferably 20～40min.
The sugared mixing speed of the headspace solid-phase microextraction is preferably 200～300rpm/min；More preferably 250～300rpm/
min。
The grams of sugar-like product is preferably 50～100g in extraction flask.
The present invention coordinates the present invention using above-mentioned extracting head, and specifically adsorption temp, time and mixing speed can be more preferable
Ground is adsorbed by the volatile component of sugar.
After the completion of absorption, in gas chromatograph-mass spectrometer injection port desorption, that is, sample introduction operation is completed.
The desorption temperature of the extracting head of the headspace solid-phase microextraction is preferably 240～250 DEG C；The desorption time is preferred
For 2～5min；More preferably 3～5min.
Volatile component is detected using gas chromatography-mass spectrum-smelling method.
The detection parameter of the gas chromatography-mass spectrum-smelling is as follows：
Chromatographic condition：Chromatographic column is HP-5 capillary chromatographic columns；1～1.2mL/min of flow rate of carrier gas；
Temperature programming is：50～55 DEG C of initial temperature, keeps 1～3min；100 are warming up to the speed of 5～6 DEG C/min～
110℃；220～240 DEG C are warmed up to the speed of 10～11 DEG C/min, 5～8min is kept；
Mass Spectrometry Conditions：Ion gun:EI sources；Electron energy 70ev；230～240 DEG C of ion source temperature；
Smelling condition：200～210 DEG C of interface temperature.
In the present invention, the chromatographic condition is preferably specially：
HP-5 capillary chromatographic columns, 30m*0.25mm*0.25 μm；Carrier gas：He；Purity 99.999%；
Flow rate of carrier gas preferably 1～1.2mL/min；More preferably 1.2mL/min；
Injector temperature is preferably 240～250 DEG C；More preferably 250 DEG C；Pressure is preferably 14.87psi；
Split sampling, split ratio is 1:1；
Temperature programming is preferably：50～53 DEG C of initial temperature, keeps 1～2min；Heated up with the speed of 5～5.5 DEG C/min
To 100～110 DEG C；220～230 DEG C are warmed up to the speed of 10 DEG C/min, 5～8min is kept；
More preferably 50 DEG C of initial temperature, keeps 1min；100 DEG C are warming up to the speed of 5 DEG C/min；With 10 DEG C/min's
Speed is warmed up to 220 DEG C, keeps 5min.
The Mass Spectrometry Conditions are preferably specially：
Ion gun:EI sources；Electron energy 70ev；Transmission line temperature is preferably 250～260 DEG C；More preferably 250 DEG C；
Preferably 230～240 DEG C of ion source temperature；More preferably 230 DEG C；Level Four bar temperature is preferably 150 DEG C；Solvent delay
Preferably 1min；Sweep limits is preferably 55～500.Scan mode：Full scan.
Olfactometry：The interface temperature of the smelling is preferably 200 DEG C.During detection, in order to prevent laboratory technician's mycteroxerosis,
It is passed through the air of moistening.
The present invention, can be with by the selection of above-mentioned chromatographic column, the control of temperature programming condition and the control of parameters
50～80 kinds of volatile components of beet sugar and cane suger are identified well, separating degree is high, good separating effect, identification knot
Fruit is accurately.
The present invention provides spectrum storehouse by instrument and existing spectrum storehouse is contrasted so as to enter to volatile component and mass spectrogram
Row Qualitative Identification；Quantitative analysis is carried out to volatile component by area normalization method, by smelling to odour intensity and type
Identified.
The present invention is preferably verified to the above results by sensory evaluation method, is preferably specially：
Dissolving 50g sugar cubes are put in 250 milliliters of wide-mouth bottles with screw lid and cover.
The sample prepared is covered into lid, is put in 50 DEG C of water-bath and is heated, while lightly rotational wobble
Bottle guarantees that solution is fully mixed in bottle.Evaluate the local flavor (smell) of 50 degree of sugar juices of bottle headspace after before processing.
The evaluation result and any peculiar smell of annotation of the local flavor (smell) of record detection sample.
Professional your sense organ of sensory evaluation personnel is to evaluate a kind of highstrung equipment thought, with above-mentioned common sense
Official's evaluation method can aid in the result of instrumental checking.
The invention provides a kind of detection method of the volatile component of sugar, including：Jing head space solid phases are micro- after sugar pretreatment
Volatile ingredient is extracted in extraction, is detected using gas chromatography-mass spectrum-smelling method；The extraction of the headspace solid-phase microextraction
The adsorption temp of head is 70～120 DEG C；Adsorption time is 5～60min；The detection parameter of the gas chromatography-mass spectrum-smelling is such as
Under：Chromatographic condition：Chromatographic column is HP-5 capillary chromatographic columns；1～1.2mL/min of flow rate of carrier gas；Temperature programming is：Initial temperature
50～55 DEG C, keep 1～3min；100～110 DEG C are warming up to the speed of 5～6 DEG C/min；With the speed of 10～11 DEG C/min
220～240 DEG C are warmed up to, 5～8min is kept；Mass Spectrometry Conditions：Ion gun:EI sources；Electron energy 70ev；Ion source temperature 230
～240 DEG C；Smelling condition：200～210 DEG C of interface temperature；By composing storehouse and area normalization method volatile component is carried out to determine
Property and quantitative analysis, are identified odour intensity and type by smelling.The present invention is directly right by headspace solid-phase microextraction
Sugar-like product are processed, concentrating volatile component, without the need for complicated pre-treatment step；Gas chromatography-mass spectrum-smelling is utilized simultaneously
Method is detected to volatile component, for volatile component while qualitative and Quantitative measurement is carried out to volatile component
Odor types and intensity have carried out synchronous identification, and method is simple, and qualification result is accurate.And compare with subjective appreciation, relatively
Prior art, closer in closer in actual naked eyes evaluation result.Carry out tracing to the source there is provided reference for product is specific.It is simultaneously right
There is highly important meaning in the difference analysis of the different product smell quality sugared for actual production and application and raising
Justice.
Odour intensity criterion：GC-O Pyatyis odour intensity method uses for reference China in following embodiment《Odor pollution
Thing discharge standard》6 grades of odor strength representations of (GB 14554-93), merge into 1 grade, so by 0 grade in the method and 1 grade
According to 2,3,4,55 grades of smell ranks and odour intensity are represented successively afterwards, following correspondence is felt in its odour intensity rank and smell：
1 can feel without any sense of smell or somewhat extremely weak smell (detection threshold concentration)；
2 can feel and tell which kind of smell (confirmation threshold concentration)；
3 can be clearly felt that scent of；
4 can feel strong smell；
5 can feel extremely strong strong smell.
In order to further illustrate the present invention, the detection of the present invention is provided sugared volatile component with reference to embodiments
Method is described in detail.
Embodiment 1
Beet sugar sugar cube is measured using following steps.Comprise the following steps that：
Crush：By beet sugar sample 120g, crushed with pulverizer ,≤the particle of 0.2mm sifted out using round-hole mesh, mixed,
It is divided into each 50g in two parts and is respectively charged into after clean container and seals,
Extract：A copy of it 50g crushing samples are put in the sample bottle of SPME injector, by 30 μm of CAR-
PDMS solid phase micro-extracting heads are inserted into the head space part of sample bottle, sample are stirred with the speed of 250rpm/min, 120
Adsorb 10min at DEG C to be collected.
Detection：Extracting head is extracted from sample bottle, the injection port for inserting gas chromatograph-mass spectrometer (GC-MS) is parsed, solved
Analysis time 2min；Sample extraction head is put into into instrument associated with GC-MS-OD to be tested, record smelt odor types and
Intensity；
Location parameter is as follows：
HP-5 capillary chromatographic columns, 30m*0.25mm*0.25 μm；Carrier gas：He；Purity 99.999%；
Flow rate of carrier gas 1.2mL/min；250 DEG C of injector temperature；Pressure 14.87psi；Split sampling, split ratio is 1:1；
Temperature programming：50 DEG C, keep 1min；100 DEG C are warming up to the speed of 5 DEG C/min；220 are warmed up to the speed of 10 DEG C/min
DEG C, keep 5min.
Ion gun:EI sources；Electron energy 70ev；250 DEG C of transmission line temperature；230 DEG C of ion source temperature；Level Four bar temperature is
150℃；Solvent delay is 1min；Sweep limits is 55～500.Scan mode：Full scan.
Olfactometry：The interface temperature of the smelling is preferably 200 DEG C.During detection, in order to prevent laboratory technician's mycteroxerosis,
It is passed through the air of moistening.
Qualitative and quantitative analysis is carried out to volatile component by composing storehouse and area normalization method, it is strong to smell by smelling
Degree and type are identified.The chromatogram for obtaining is as shown in figure 1, Fig. 1 is the GC-MS figures of the detection of the embodiment of the present invention 1；Concrete group
Divide as shown in table 2, table 2 is the volatile component table of the detection of the embodiment of the present invention 1；
Contrast sensory testing：Heated at other a 50g sugar sample bottle is put into into 50 DEG C, carried out sensory test, remembered
The measured odor types of record.Local flavor (smell) per ten minutes to solution carries out evaluating no less than 30 minutes, and record surveys result.
Table 2 is the volatile component table of the detection of the embodiment of the present invention 1
Embodiment 2
Cane suger sugar cube is measured using following steps.Comprise the following steps that：
Crush：By cane suger sample 120g, crushed with pulverizer ,≤the particle of 0.2mm sifted out using round-hole mesh, mixed,
It is divided into each 50g in two parts and is respectively charged into after clean container and seals,
Extract：A copy of it 50g crushing samples are put in the sample bottle of SPME injector, by 30 μm of CAR-
PDMS solid phase micro-extracting heads are inserted into the head space part of sample bottle, sample are stirred with the speed of 250rpm/min, 70
Adsorb 1min at DEG C to be collected.
Detection：Extracting head is extracted from sample bottle, the injection port for inserting gas chromatograph-mass spectrometer (GC-MS) is parsed, solved
Analysis time 2min.Sample extraction head is put into into instrument associated with GC-MS-OD to be tested, record smelt odor types and
Intensity；Location parameter is with embodiment 1
Qualitative and quantitative analysis is carried out to volatile component by composing storehouse and area normalization method, it is strong to smell by smelling
Degree and type are identified that the chromatogram for obtaining such as Fig. 2 shows, the GC-MS figures of the detection of Fig. 2 embodiment of the present invention 2；Concrete component is such as
Table 3 shows that table 3 is the volatile component table of the detection of the embodiment of the present invention 2；
Contrast sensory testing：Heated at other a 50g sugar sample bottle is put into into 50 DEG C, carried out sensory test, remembered
The measured odor types of record.Local flavor (smell) per ten minutes to solution carries out evaluating no less than 30 minutes, and record surveys result.
Table 3 is the volatile component table of the detection of the embodiment of the present invention 2
Embodiment 3
Cane suger sugar cube is measured using following steps.Comprise the following steps that：
Crush：By cane suger sample 120g, crushed with pulverizer ,≤the particle of 0.2mm sifted out using round-hole mesh, mixed,
It is divided into each 50g in two parts and is respectively charged into after clean container and seals,
Extract：A copy of it 50g crushing samples are put in the sample bottle of SPME injector, by 30 μm of CAR-
PDMS solid phase micro-extracting heads are inserted into the head space part of sample bottle, sample are stirred with the speed of 250rpm/min, 120
Adsorb 20min at DEG C to be collected.
Detection：Extracting head is extracted from sample bottle, the injection port for inserting gas chromatograph-mass spectrometer (GC-MS) is parsed, solved
Analysis time 5min.Sample extraction head is put into into instrument associated with GC-MS-OD to be tested, record smelt odor types and
Intensity；Location parameter is with embodiment 1
Qualitative and quantitative analysis is carried out to volatile component by composing storehouse and area normalization method, it is strong to smell by smelling
Degree and type are identified that the chromatogram for obtaining such as Fig. 3, Fig. 3 scheme for the GC-MS of the embodiment of the present invention 3；Concrete component such as table 4,
Table 4 is the volatile component table of the detection of the embodiment of the present invention 3；
Contrast sensory testing：Heated at other a 50g sugar sample bottle is put into into 50 DEG C, carried out sensory test, remembered
The measured odor types of record.Comparative example is carried out evaluating no less than 30 points by the local flavor (smell) per ten minutes to solution with real
Clock, record surveys result.
Table 4 is the volatile component table of the detection of the embodiment of the present invention 3
Comparative example 1
Beet sugar sugar cube is measured using following steps.The method of reference literature is to aroma compound in beet sugar
Identification (Marsili, Journal of Chromatographic Science, 1994,32:165-171.) and using test
The step is processed sample, and is collected smell and processed.
Comprise the following steps that：
Dissolving：Beet sugar sample 120g and 2gNaCl are placed in 500mL solvent bottles, solid sample is entered with 150ml water
Row dissolving.
Purging：Bottle is put into into water-bath, 45 DEG C are heated to, and with hot-air being passed through in conduit, is stretched into sugar juice and is blown
75min is swept, purged hot-air is into a gas trap for filling charcoal absorption adsorbent.
Parsing：The gas trap that will be filled with adsorbent is heated to 210 DEG C, continues to blow with the flow velocity of 60mL/min with helium
15min is swept, and escaping gas is collected with second adsorbed gas trap, and open dewatering cycle, at 40 DEG C
Lower purging 4min eliminates moisture interference.
Analysis：Then 10min is purged at second trap being placed on into 210 DEG C, the escaping gas for being blown out enters gas
Chromatography is analyzed；The GC-MS figures of the chromatogram for obtaining such as Fig. 4, Fig. 4 comparative example 1 of the present invention；The concrete component such as institute of table 5
Show, table 5 is the volatile component table of the detection of comparative example of the present invention 1；
Contrast sensory testing：Heated at 50g sugar sample bottles are put into into 50 DEG C, carried out sensory test, record is measured
Odor types.Local flavor (smell) per ten minutes to solution carries out evaluating no less than 30 minutes, and record surveys result.As a result such as table
Shown in 1, table 1 is the sensory test result of the embodiment of the present invention and comparative example.
Table 1 is the sensory test result of the embodiment of the present invention and comparative example
Table 5 is the volatile component table of the detection of comparative example of the present invention 1
Contrasted by table 1, table 2 and table 5 as can be seen that the smell qualification result of the present invention is closer in actual naked eyes evaluation knot
Really.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. it is a kind of sugar volatile component detection method, it is characterised in that include：
Jing headspace solid-phase microextractions extract volatile ingredient after sugar pretreatment, are examined using gas chromatography-mass spectrum-smelling method
Survey；
The adsorption temp of the extracting head of the headspace solid-phase microextraction is 70～120 DEG C；Adsorption time is 5～60min；
The detection parameter of the gas chromatography-mass spectrum-smelling is as follows：
Chromatographic condition：Chromatographic column is HP-5 capillary chromatographic columns；1～1.2mL/min of flow rate of carrier gas；
Temperature programming is：50～55 DEG C of initial temperature, keeps 1～3min；100～110 are warming up to the speed of 5～6 DEG C/min
℃；220～240 DEG C are warmed up to the speed of 10～11 DEG C/min, 5～8min is kept；
Mass Spectrometry Conditions：Ion gun:EI sources；Electron energy 70ev；230～240 DEG C of ion source temperature；
Smelling condition：200～210 DEG C of interface temperature；
Qualitative and quantitative analysis is carried out to volatile component by composing storehouse and area normalization method, by smelling to odour intensity and
Type is identified.
2. detection method according to claim 1, it is characterised in that the absorption of the extracting head of the headspace solid-phase microextraction
Temperature is 80～120 DEG C；Adsorption time is 15～45min.
3. detection method according to claim 1, it is characterised in that the extracting head of the headspace solid-phase microextraction is extraction
Fiber, the extracting fiber is DVB/CAR/PDMS；Carrier thickness is 30～50 μm.
4. detection method according to claim 1, it is characterised in that the sugared mixing speed of the headspace solid-phase microextraction
For 200～300rpm/min.
5. detection method according to claim 1, it is characterised in that the desorption of the extracting head of the headspace solid-phase microextraction
Temperature is 240～250 DEG C；The desorption time is 2～5min.
6. detection method according to claim 1, it is characterised in that the chromatographic condition is specially：
HP-5 capillary chromatographic columns, 30m*0.25mm*0.25 μm；Carrier gas：He；1～1.2mL/min of flow rate of carrier gas；Injection port temperature
Spend for 240～250 DEG C；Split sampling, split ratio is 1:1；
Temperature programming is：50～53 DEG C of initial temperature, keeps 1～2min；100 are warming up to the speed of 5～5.5 DEG C/min～
110℃；220～230 DEG C are warmed up to the speed of 10 DEG C/min, 5～8min is kept.
7. detection method according to claim 1, it is characterised in that the Mass Spectrometry Conditions are specially：
Ion gun:EI sources；Electron energy 70ev；250～260 DEG C of transmission line temperature；230～240 DEG C of ion source temperature；Level Four bar
Temperature is 150 DEG C；Solvent delay 1min；Sweep limits 55～500.
8. detection method according to claim 1, it is characterised in that the interface temperature of the smelling is 200 DEG C.
9. detection method according to claim 1, it is characterised in that the sugar is including the one kind in beet sugar and cane suger
Or it is several.
10. detection method according to claim 1, it is characterised in that the pretreatment of the sugar to crush, the granularity of crushing
It is less than 0.2mm.
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| CN113125578A (en) * | 2019-12-31 | 2021-07-16 | 中粮集团有限公司 | Identification and analysis method of flavor components of colored sugar |
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