CN108828093A - Headspace solid-phase microextraction-Gc-mss method of volatile component in a kind of pueraria lobata - Google Patents
Headspace solid-phase microextraction-Gc-mss method of volatile component in a kind of pueraria lobata Download PDFInfo
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- pueraria lobata
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- 235000010575 Pueraria lobata Nutrition 0.000 title claims abstract description 41
- 241000219781 Pueraria montana var. lobata Species 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000007790 solid phase Substances 0.000 title claims abstract description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- 239000000284 extract Substances 0.000 claims abstract description 7
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 7
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 4
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 8
- 238000003795 desorption Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 4
- 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 4
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000575 pesticide Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004853 microextraction Methods 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims 1
- 239000004615 ingredient Substances 0.000 abstract description 6
- 241000219780 Pueraria Species 0.000 abstract description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000000341 volatile oil Substances 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- ZQSIJRDFPHDXIC-UHFFFAOYSA-N daidzein Chemical compound C1=CC(O)=CC=C1C1=COC2=CC(O)=CC=C2C1=O ZQSIJRDFPHDXIC-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 235000018927 edible plant Nutrition 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- -1 flavone compounds Chemical class 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 2
- FLIACVVOZYBSBS-UHFFFAOYSA-N Methyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC FLIACVVOZYBSBS-UHFFFAOYSA-N 0.000 description 2
- RXUWDKBZZLIASQ-UHFFFAOYSA-N Puerarin Natural products OCC1OC(Oc2c(O)cc(O)c3C(=O)C(=COc23)c4ccc(O)cc4)C(O)C(O)C1O RXUWDKBZZLIASQ-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000035622 drinking Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- XIRNKXNNONJFQO-UHFFFAOYSA-N ethyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCC XIRNKXNNONJFQO-UHFFFAOYSA-N 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 235000008216 herbs Nutrition 0.000 description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 2
- 235000020778 linoleic acid Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- HKEAFJYKMMKDOR-VPRICQMDSA-N puerarin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=CC(C2=O)=C1OC=C2C1=CC=C(O)C=C1 HKEAFJYKMMKDOR-VPRICQMDSA-N 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- YVBAUDVGOFCUSG-UHFFFAOYSA-N 2-pentylfuran Chemical class CCCCCC1=CC=CO1 YVBAUDVGOFCUSG-UHFFFAOYSA-N 0.000 description 1
- 208000007848 Alcoholism Diseases 0.000 description 1
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- GMTUGPYJRUMVTC-UHFFFAOYSA-N Daidzin Natural products OC(COc1ccc2C(=O)C(=COc2c1)c3ccc(O)cc3)C(O)C(O)C(O)C=O GMTUGPYJRUMVTC-UHFFFAOYSA-N 0.000 description 1
- KYQZWONCHDNPDP-UHFFFAOYSA-N Daidzoside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C2C(=O)C(C=3C=CC(O)=CC=3)=COC2=C1 KYQZWONCHDNPDP-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000019695 Migraine disease Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229930186706 Puerarin-xyloside Natural products 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 201000007930 alcohol dependence Diseases 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 235000007240 daidzein Nutrition 0.000 description 1
- KYQZWONCHDNPDP-QNDFHXLGSA-N daidzein 7-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C2C(=O)C(C=3C=CC(O)=CC=3)=COC2=C1 KYQZWONCHDNPDP-QNDFHXLGSA-N 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FMMOOAYVCKXGMF-MURFETPASA-N ethyl linoleate Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(=O)OCC FMMOOAYVCKXGMF-MURFETPASA-N 0.000 description 1
- 229940031016 ethyl linoleate Drugs 0.000 description 1
- 229940067592 ethyl palmitate Drugs 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 230000012447 hatching Effects 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- CJWQYWQDLBZGPD-UHFFFAOYSA-N isoflavone Natural products C1=C(OC)C(OC)=CC(OC)=C1C1=COC2=C(C=CC(C)(C)O3)C3=C(OC)C=C2C1=O CJWQYWQDLBZGPD-UHFFFAOYSA-N 0.000 description 1
- 235000008696 isoflavones Nutrition 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- FMMOOAYVCKXGMF-UHFFFAOYSA-N linoleic acid ethyl ester Natural products CCCCCC=CCC=CCCCCCCCC(=O)OCC FMMOOAYVCKXGMF-UHFFFAOYSA-N 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 230000005906 menstruation Effects 0.000 description 1
- QETDZFXKONOEOC-UHFFFAOYSA-N methyl octadeca-7,10-dienoate Chemical class CCCCCCCC=CCC=CCCCCCC(=O)OC QETDZFXKONOEOC-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- GGHMUJBZYLPWFD-CUZKYEQNSA-N patchouli alcohol Chemical compound C1C[C@]2(C)[C@@]3(O)CC[C@H](C)[C@@H]2C[C@@H]1C3(C)C GGHMUJBZYLPWFD-CUZKYEQNSA-N 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- NAAXIGQVODQJOV-PXYOAQHISA-N puerarin xyloside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C(C1=C(C(C(C=2C=CC(O)=CC=2)=CO1)=O)C=C1)=C1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)CO1 NAAXIGQVODQJOV-PXYOAQHISA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- GGHMUJBZYLPWFD-UHFFFAOYSA-N rac-patchouli alcohol Natural products C1CC2(C)C3(O)CCC(C)C2CC1C3(C)C GGHMUJBZYLPWFD-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- 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 discloses a kind of headspace solid-phase microextraction of volatile component in pueraria lobata-Gc-mss methods, it includes the following steps：(1) headspace solid-phase microextraction extracts volatile component；(2) gas chromatography-mass spectrography analysis condition：Chromatographic condition：40 DEG C of capillary chromatographic column initial temperature, 1min is kept, is then warming up to 200 DEG C with the rate of 5 DEG C/min, keeps 2min, then be warming up to 250 DEG C with the rate of 15 DEG C/min and keep 2min；Injector temperature is 250 DEG C；Mass Spectrometry Conditions：Ion source：EI ion source；Ion source temperature：280℃；Transmission line temperature：280℃；Electron bombardment energy：70eV；Scanning mode：Full scan；Mass scan range：35~400m/z；Qualitative and quantitative analysis is carried out to the mass spectrometric data of finally obtained volatile component.The present invention identifies wherein 67 kinds of ingredients by the isolated 91 kinds of pueraria lobata components of headspace solid-phase microextraction-gas chromatography mass spectrometry method.
Description
Technical field
The present invention relates to a kind of headspace solid-phase microextraction of volatile component in pueraria lobata-Gc-mss methods.
Background technique
Pueraria lobata (Pueraria lobata) is the drying of legume pueraria lobata (Pueraria lobata Willd Ohwi)
Root, main plantation is in Henan, Hebei, Hunan, Liaoning, Guangdong, zhejiang and other places.Pueraria lobata starch rich in, dietary fiber, sugar
The substances such as class, also containing there are many flavone compounds, such as daidzein, Puerarin, daidzin, Puerarin xyloside.《Legendary god of farming's sheet
Grass warp》It is sweet in flavor, pungent to record its, it is cool.Returns spleen, stomach, lung channel.There is expelling pathogenic factors from muscles and skin to bring down a fever, promotes the production of body fluid to quench thirst, promoting eruption, Shengyang Zhixie, promoting menstruation work
Network, relieving alcoholism and other effects.Modern pharmacological studies have shown that pueraria lobata, which has, improves cardiovascular and cerebrovascular disease, hypoglycemic, reducing blood lipid, resist swollen
Tumor, the effects of relieving the effect of alcohol, clinically can be used for treating hypertension, angina pectoris, coronary heart disease, migraines, diabetes, enteron aisle lesion etc.
Disease.
Pueraria polysaccharide, Puerarin, isoflavone compound are concentrated mainly on to the research and development of pueraria lobata both at home and abroad at present
Extract etc., and researching and analysing for its volatile chemical component is rarely reported.
Summary of the invention
The purpose of the present invention is to provide a kind of headspace solid-phase microextraction-Gc-mss of volatile component in pueraria lobata
Method, it includes the following steps：
(1) headspace solid-phase microextraction extracts volatile component
It weighs pueraria lobata to be placed in ml headspace bottle, 50~90 DEG C of 4~16min of balance, by 50/30 μm of DVB/CAR/PDMS solid phase
Micro-extracting head is inserted into 30~60min of extraction absorption in ml headspace bottle, takes out, is immediately inserted into gas chromatographic sample introduction mouth, solves at 250 DEG C
Inhale 3~9min；
(2) gas chromatography-mass spectrography analysis condition
Chromatographic condition：40 DEG C of capillary chromatographic column initial temperature, 1min is kept, is then warming up to the rate of 5 DEG C/min
200 DEG C, 2min is kept, then be warming up to 250 DEG C with the rate of 15 DEG C/min and keep 2min；Injector temperature is 250 DEG C；
Mass Spectrometry Conditions：Ion source：EI ion source；Ion source temperature：280℃；Transmission line temperature：280℃；Electron bombardment energy
Amount：70eV；Scanning mode：Full scan；Mass scan range：35~400m/z；
Qualitative and quantitative analysis is carried out to the mass spectrometric data of finally obtained volatile component.
Further, in rapid (1), the temperature when balance is 70~90 DEG C, preferably 90 DEG C.
Further, in step (1), the time of the balance is 13min.
Further, in step (1), the time of the extraction absorption is 40~60min, preferably 50min.
Further, in step (1), the time of the desorption is 3~7min, preferably 5min.
Further, in step (1), the solid phase micro-extracting head is before extracting pueraria lobata volatile component at 270 DEG C
Aging process 30min.
Further, in step (2), the chromatographic column is TR-PESTICIDE elastic quartz capillary column, having a size of 30m
×0.25mm×0.25μm。
Further, in step (2), carrier gas is 99.999% high-purity helium；Flow velocity 1.2mL/min；Split ratio is 10:
1。
The present invention is identified by the isolated 91 kinds of pueraria lobata components of headspace solid-phase microextraction-gas chromatography mass spectrometry method
Wherein 67 kinds of ingredients.Li Yaohua etc. using extraction by steam distillation Sichuan, Hunan, volatile oil in the place of production pueraria lobata of three, Guangxi,
And each place of production pueraria lobata volatile oil compositions are detected with gas chromatograph-mass spectrometer (GC-MS), three place of production pueraria lobatas volatilize oil as the result is shown
Do not identify 20,24,21 kind of component and content it is highest be linoleic acid.Through it was found that, the pueraria lobata that this research identifies is waved
It is significant superior to illustrate that detection method and qualitative analysis means of the invention have far more than above-mentioned document report for hair property ingredient
Property.And method high degree of automation of the invention, it is easy to operate, qualitative it is more accurate, result is relatively reliable, can also apply
Into the detection and analysis of other medicinal and edible plant volatile components, for the quality for controlling medicinal and edible plant, promote integration of drinking and medicinal herbs
The development of industry provides scientific support.
Obviously, above content according to the present invention is not being departed from according to the ordinary technical knowledge and customary means of this field
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The specific embodiment of form by the following examples remakes further specifically above content of the invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to example below.It is all to be based on above content of the present invention
The technology realized all belongs to the scope of the present invention.
Detailed description of the invention
Fig. 1 is the total ion current figure of pueraria lobata volatile materials ingredient.
Specific embodiment
The detection and analysis of embodiment 1, pueraria lobata volatile component
1 material and reagent
The dry medicinal material of pueraria lobata originates from Guangxi province, Zhong Zhi great pharmacy chain Co., Ltd of Zhongshan city；N-alkane hybrid standard product
(C7~C40), o2si company of the U.S.
2 instrument and equipments
(GC-MS/MS matches electron ionization sources and Xcalibur to triple level four bars series connection matter connection instrument to 8000 gas-chromatography of TSQ-
Data processing system), TRIPLUS RSH autosampler, 20mL headspace sample bottle, solid phase microextraction automatic sampling handle, beauty
Thermo company of state；50/30 μm of DVB/CAR/PDMS solid phase micro-extracting head, Supelco company of the U.S..
3 experimental methods
3.1 Headspace solid phase microextractiom
It accurately weighs pueraria lobata fragment 3.0g and is placed in 20mL ml headspace bottle (thread sealed closure equipped with polytetrafluoroethylene (PTFE) pad), from
Ml headspace bottle is placed in 90 DEG C of hatching furnace after balance 13min, by (the aging at 270 DEG C of injection port of aging by dynamic sample injector
50/30 μm of DVB/CAR/PDMS solid phase micro-extracting head 30min) is rapidly inserted into sample bottle head space part and carries out extracting hot absorption
Then extracting head after absorption is inserted into gas chromatographic sample introduction mouth, desorbs 5min under the conditions of 250 DEG C, finally enter by 50min
GC-MS/MS system carries out separation detection.
The analysis of 3.2 gas chromatography-mass spectrographies
Chromatographic condition：TR-PESTICIDE elastic quartz capillary column (30m × 0.25mm, 0.25 μm)；Temperature program：Initially
40 DEG C of temperature, 1min is kept, is then warming up to 200 DEG C with the rate of 5 DEG C/min, keeps 2min, then with the rate of 15 DEG C/min
It is warming up to 250 DEG C and keeps 2min；Split ratio 10：1；Injector temperature is 250 DEG C；Carrier gas：99.999% high-purity helium；Stream
Fast 1.2mL/min.
Mass Spectrometry Conditions：EI ion source；Ion source temperature：280℃；Transmission line temperature：280℃；Electron bombardment energy：
70eV；Scanning mode：Full scan；35~400m/z of mass scan range.
The qualitative and quantitative analysis of 3.3 volatile components
Using automatic mass spectrum deconvolution qualitative systems (AMDIS) to volatile materials total ion current figure (TIC) in pueraria lobata from
Dynamic to carry out deconvolution processing, the mass spectrum differentiated is retrieved in NIST2.2 standard spectrum library, according to matching degree, retention index and text
It offers and has reported that substance is checked, positive match and counter-match is only selected to be all larger than 800 substance, and with areas of peak normalization method meter
Calculate the relative amount of each volatile materials of pueraria lobata.
Retention index, which is that C7~C40 n-alkane is mixed, to be marked under analysis condition identical with pueraria lobata sample after sample introduction, automatically
Mass spectrum deconvolution qualitative systems (AMDIS) calculate the reservation of each volatile component according to the retention time of n-alkane automatically
Index.
3.4 testing result
The volatile component of 1 pueraria lobata of table
The total ion current figure of volatile materials ingredient is shown in that Fig. 1, volatile component and percentage contents are as shown in table 1.Pueraria lobota
Root volatile component total ion current figure isolates to obtain 91 kinds of components, and identifies wherein 67 kinds of ingredients, and it is total to account for volatile materials
The 88.91% of amount, including olefines, aldehydes, esters, alcohols, ketone and other class compounds.Wherein, it is ester that content is highest
Class has 11 kinds, accounts for the 26.05% of volatile materials total amount；Followed by aldehydes 22 (22.16%), alcohols 9 (13.85%),
Ketone 5 (5.59%), terpenes 8 (2.88%).In addition content 10 is from high in the end successively Patchoulicalcohol before ranking
(9.72%), ethyl palmitate (7.63%), isoesdragol (6.61%), furfural (5.93%), ethyl linoleate (4.80%),
Acetic acid (4.28%), 7,10- octadecadienoic acid methyl esters (3.70%), methyl palmitate (3.64%), hexanal (3.60%) and
2- n-pentyl furans (3.58%), accounts for the 53.49% of volatile component total amount.
The pueraria lobata volatile component and other document reports that the present invention identifies have different.Li Yaohua etc. is steamed using water
Steam distillation method extracts Sichuan, Hunan, volatile oil in the place of production pueraria lobata of three, Guangxi, and is detected with gas chromatograph-mass spectrometer (GC-MS) each
Place of production pueraria lobata volatile oil compositions, as the result is shown three place of production pueraria lobata volatile oil identify 20 respectively, 24,21 kind of component and content most
High is linoleic acid.Through it was found that, the pueraria lobata volatile component that the present invention identifies is far more than above-mentioned document report, explanation
The detection method and qualitative analysis means have significant superiority.
The screening of embodiment 2, head space micro-extraction condition
Since the effect of extracting of Headspace-solid phase microextraction method is by conditions such as extraction adsorption time, extraction temperature, desorption times
Influence, the present invention by choose volatile materials total peak area and total peak number mesh be inspection target, compare different extractions
The influence of adsorption time, extraction temperature, desorption time to pueraria lobata volatile materials effect of extracting is taken, and determines Optimal Parameters.
Experimental method is carried out according to embodiment 1, wherein extraction adsorption time, extraction temperature, desorption time are selected by table 2,
The influence of difference extraction adsorption time, extraction temperature, desorption time to pueraria lobata volatile materials effect of extracting the results are shown in Table 2.
Influence of the different factors of table 2 to pueraria lobata volatile materials effect of extracting
As it can be seen from table 1 the more excellent condition of Headspace solid phase microextractiom extraction pueraria lobata volatile component is：Extraction temperature
For 90 DEG C, extraction adsorption time 50min, desorption time 5min.
To sum up, the present invention has determined that Headspace-solid phase microextraction method extracts pueraria lobata volatile component by multifactorial experiment
Preferable parameter, and the pueraria lobata volatile materials that extracts under the conditions of preferably is detected using combined gas chromatography mass spectrometry, benefit
Qualitative analysis is carried out to its component with automatic deconvolution technique (AMDIS) and retention index, 67 kinds of compounds is finally identified, is
Theoretical basis has been established in the development of pueraria lobata industry.And it is method high degree of automation of the invention, easy to operate, qualitative more quasi-
Really, result is relatively reliable, also can be applied in the detection and analysis of other medicinal and edible plant volatile components, same for control medicine food
The quality of source plant promotes the development of integration of drinking and medicinal herbs industry to provide scientific support.
Claims (8)
1. the headspace solid-phase microextraction of volatile component-Gc-mss method in a kind of pueraria lobata, it is characterised in that：It include with
Lower step：
(1) headspace solid-phase microextraction extracts volatile component
It weighs pueraria lobata to be placed in ml headspace bottle, 50~90 DEG C of 4~16min of balance, by 50/30 μm of micro- extraction of DVB/CAR/PDMS solid phase
Extraction 30~60min of absorption in head insertion ml headspace bottle is taken, is taken out, is immediately inserted into gas chromatographic sample introduction mouth, desorbs 3 at 250 DEG C
~9min；
(2) gas chromatography-mass spectrography analysis condition
Chromatographic condition：40 DEG C of capillary chromatographic column initial temperature, 1min is kept, is then warming up to 200 with the rate of 5 DEG C/min
DEG C, 2min is kept, then be warming up to 250 DEG C with the rate of 15 DEG C/min and keep 2min；Injector temperature is 250 DEG C；
Mass Spectrometry Conditions：Ion source：EI ion source；Ion source temperature：280℃；Transmission line temperature：280℃；Electron bombardment energy：
70eV；Scanning mode：Full scan；Mass scan range：35~400m/z；
Qualitative and quantitative analysis is carried out to the mass spectrometric data of finally obtained volatile component.
2. according to the method described in claim 1, it is characterized in that：In step (1), the temperature when balance is 70~90
DEG C, preferably 90 DEG C.
3. method according to claim 1 or 2, it is characterised in that：In step (1), the time of the balance is 13min.
4. described in any item methods according to claim 1~3, it is characterised in that：In step (1), it is described extraction absorption when
Between be 40~60min, preferably 50min.
5. method according to any one of claims 1 to 4, it is characterised in that：In step (1), the time of the desorption is 3
~7min, preferably 5min.
6. described in any item methods according to claim 1~5, it is characterised in that：In step (1), the solid phase micro-extracting head
Before extracting pueraria lobata volatile component at 270 DEG C aging process 30min.
7. described in any item methods according to claim 1~6, it is characterised in that：In step (2), the chromatographic column is TR-
PESTICIDE elastic quartz capillary column, having a size of 30m × 0.25mm × 0.25 μm.
8. described in any item methods according to claim 1~7, it is characterised in that：In step (2), carrier gas is 99.999% high
Purity helium；Flow velocity 1.2mL/min；Split ratio is 10:1.
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