CN106442824A - Gas Chromatographic Method for Detecting C18 Fatty Acid in Oil - Google Patents
Gas Chromatographic Method for Detecting C18 Fatty Acid in Oil Download PDFInfo
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- CN106442824A CN106442824A CN201610853228.4A CN201610853228A CN106442824A CN 106442824 A CN106442824 A CN 106442824A CN 201610853228 A CN201610853228 A CN 201610853228A CN 106442824 A CN106442824 A CN 106442824A
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- Prior art keywords
- grease
- acid isomer
- fat acid
- slb
- ionic liquid
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Links
- 239000000194 fatty acid Substances 0.000 title claims abstract description 13
- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 12
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 12
- 150000004665 fatty acids Chemical class 0.000 title claims abstract description 12
- 238000004587 chromatography analysis Methods 0.000 title description 6
- 238000001514 detection method Methods 0.000 claims abstract description 38
- 239000004519 grease Substances 0.000 claims abstract description 38
- 239000002608 ionic liquid Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000004817 gas chromatography Methods 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims description 53
- 239000007789 gas Substances 0.000 claims description 30
- 238000010792 warming Methods 0.000 claims description 18
- 210000000481 breast Anatomy 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000012086 standard solution Substances 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 11
- 238000002203 pretreatment Methods 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 9
- 239000008158 vegetable oil Substances 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 claims description 8
- 239000010775 animal oil Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- NDJUHNMZOYJNTF-UHFFFAOYSA-N CO.ClCC(=O)Cl Chemical compound CO.ClCC(=O)Cl NDJUHNMZOYJNTF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 230000009514 concussion Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 238000001228 spectrum Methods 0.000 claims 1
- 238000004445 quantitative analysis Methods 0.000 abstract description 13
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical class CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 abstract description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 abstract description 7
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical class CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 abstract description 2
- 239000003925 fat Substances 0.000 description 22
- 235000019197 fats Nutrition 0.000 description 22
- 125000001931 aliphatic group Chemical group 0.000 description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000003921 oil Substances 0.000 description 7
- 235000019198 oils Nutrition 0.000 description 7
- 235000012424 soybean oil Nutrition 0.000 description 6
- 239000003549 soybean oil Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 239000002285 corn oil Substances 0.000 description 5
- 235000005687 corn oil Nutrition 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 235000004347 Perilla Nutrition 0.000 description 4
- 244000124853 Perilla frutescens Species 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000004451 qualitative analysis Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 235000021149 fatty food Nutrition 0.000 description 3
- 235000021388 linseed oil Nutrition 0.000 description 3
- 239000000944 linseed oil Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 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
- 235000013336 milk Nutrition 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- DYLIWHYUXAJDOJ-OWOJBTEDSA-N (e)-4-(6-aminopurin-9-yl)but-2-en-1-ol Chemical compound NC1=NC=NC2=C1N=CN2C\C=C\CO DYLIWHYUXAJDOJ-OWOJBTEDSA-N 0.000 description 1
- 240000006240 Linum usitatissimum Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 235000019486 Sunflower oil Nutrition 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012482 calibration solution Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- -1 cyanogen propyl-siloxane Chemical class 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 235000010692 trans-unsaturated fatty acids Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 239000002699 waste material 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- 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
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)
- Fats And Perfumes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a gas chromatography method for detecting C18 fatty acid isomers in grease. A high-polarity ionic liquid gas chromatographic column with the specifications of 200 m*0.25 mm*0.20 mu m is used for detecting the C18 fatty acid isomers in the grease. By means of the method, the separation degree of C18:1 and C18:2 isomers is improved and C18:3 isomers are effectively separated. According to the established C18 fatty acid isomer method, the RSD (relative standard deviation) of the within-day precision is controlled in the range of 0.83%-4.30%, the RSD of the day to day precision is controlled in the range of 1.53%-3.90%, and the quantitative analysis requirements are met. According to the established C18 fatty acid isomer method, the detection limit ranges from 0.009 mg/L to 0.075 mg/L, and the minimum determination limit ranges from 0.028 mg/L to 0.225 mg/L, and the detection limit and the determination limit of C18 cis-trans-isomers are remarkably reduced.
Description
Technical field
The present invention relates to grease detection technique field, particularly to a kind of gas-chromatography of C18 aliphatic acid in detection grease
Method.
Background technology
In daily life, all can take in fatty foods daily, but process vegetable oil used by these food, animal oil or
Animal breast, such as soybean oil, rapeseed oil, sunflower oil, lard or milk etc. can produce trans-fatty acid in pyroprocess, particularly
The frying oil of waste oil category is used for culinary art and the processing of food by many illegal retailers, contained anti-in a large number in these poor oils
Formula aliphatic acid causes serious harm to the nutrient health of consumer, and the trans fats acid isomer in high-temperature vegetable oil mainly comes
Come from C18 unrighted acid.
C18 unrighted acid in vegetable fat is oleic acid, linoleic acid plus linolenic acid, and isomery can occur after high-temperature heating
Change reaction, generate antiform oleic acid, trans-linoleic acid, trans flax acid isomer.At present, detection C18 fat acid isomer is commonly used
Analysis method have infra-red sepectrometry, gas chromatography, GC-MS, silver ion thin-layered chromatography and silver ion efficient
Liquid chromatography etc..But due to C18 fat acid isomer physicochemical property closely, conventional fatty acid analysis method is difficult to
Isomers are kept completely separate and come.
The inspection that gas chromatography is widely used in fatty acid isomer in vegetable oil because separative efficiency is high, test limit is low
Survey, but these recommend SP-2560, CP-Sil 88, the gas-chromatography such as Agilent HP 88, SP-2340 and BPX-70
C18 fat acid isomer all cannot be kept completely separate by post.With deepening continuously of research, C18 fat acid isomer is latent to health
Harm and benefit obtained increasing research confirm, also result in the great attention of international community and the Chinese government.
Therefore, above cyanogen propyl-siloxane chromatographic column is replaced using up-to-date highly polar ionic liquid gas chromatographic column, to C18 in vegetable oil
Fatty acid isomer is effectively separated, and realizes the qualitative and quantitative analysis of each isomers, has potential using value.
Content of the invention
It is an object of the invention to solution at least the above, and provide the advantage that at least will be described later.
It is a still further object of the present invention to provide a kind of application specification be 200m × 0.25mm × 0.20 μm highly polar from
The gas chromatography of C18 fat acid isomer in sub- liquid gas phase SLB-IL111 chromatogram post detection grease.
In order to realize according to object of the present invention and further advantage, there is provided C18 aliphatic acid in a kind of detection grease
The gas chromatography of isomers, applies C18 aliphatic acid in highly polar ionic liquid gas phase SLB-IL111 chromatogram post detection grease different
Structure body；Wherein, the specification of highly polar ionic liquid gas phase SLB-IL111 chromatographic column is 200m × 0.25mm × 0.20 μm.
Preferably, wherein, apply C18 aliphatic acid in highly polar ionic liquid gas phase SLB-IL111 chromatogram post separation grease
Chromatographic condition during isomers is：
Injector temperature：200-230℃；Sample size：1μL；Split ratio：60-100:1；
Chromatographic column initial temperature is 60-80 DEG C, after retaining 5min, is warming up to 175 DEG C with 10-20 DEG C/min, then
Retain 15-30min, then be warming up to 185 DEG C with 1-5 DEG C/min, retain 15-70min；
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
Preferably, wherein, apply C18 aliphatic acid in highly polar ionic liquid gas phase SLB-IL111 chromatogram post separation grease
Chromatographic condition during isomers is：
Injector temperature：230℃；Sample size：1μL；Split ratio：60:1；
Chromatographic column initial temperature is 60 DEG C, after retaining 5min, is warming up to 175 DEG C with 20 DEG C/min, then retains 15min, then
It is warming up to 185 DEG C with 1 DEG C/min, retain 70min；
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
Preferably, wherein, also include pre-treatment：
1) weigh 200mg grease to be placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution；
2) add the potassium hydroxide methanol solution of 0.1mL2-5mol/L, vortex mixes 30s；
3) 10min is centrifuged with 4000rpm, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtain detection sample；
4) detection sample is isolated C18 aliphatic acid therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column different
Structure body.
Preferably, wherein, also include pre-treatment：
1) weigh 200mg grease to be placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution；
2) add the potassium hydroxide methanol solution of 0.1mL2mol/L, vortex mixes 30s；
3) 10min is centrifuged with 4000rpm, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtain detection sample；
4) detection sample is isolated C18 aliphatic acid therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column different
Structure body.
Preferably, wherein, between 0.009～0.075mg/L, minimum measures the detection limit of C18 fat acid isomer
Limit is between 0.028～0.225mg/L.
Preferably, wherein, described grease is animal oil or vegetable oil.
Preferably, wherein, described grease is animal breast, and the pre-treating method of described animal breast is：
1) weigh 200mg animal breast to be respectively placed in 10mL centrifuge tube, be added thereto to the C11 of 2mL:0 internal standard solution and 3mL
Toluene, adds the chloroacetic chloride methanol solution of 4mL10%, nitrogen charging 1min, and vortex mixes in 80 DEG C of water-bath 2h, every 20min concussion
Once；
2), after taking-up 10mL centrifuge tube is cooled to room temperature, material in 10mL centrifuge tube is transferred in 30mL centrifuge tube I, point
Do not dissolve and wash away 3 times afterwards with the sodium carbonate of 3mL 6%, liquid will be dissolved and washed away and be incorporated in 30mL centrifuge tube II, mix, 5000r/min from
Heart 5min, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtains detection sample；
3) detection sample is isolated C18 aliphatic acid therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column different
Structure body.
The present invention at least includes following beneficial effect：
(1) present invention improves C18 using the method that highly polar ionic liquid chromatographic column is set up:1 and C18:2 isomers point
From degree, and achieve C18:The efficiently separating of 3 Isomers；
(2) present invention set up C18 fat acid isomer method withinday precision control RSD be 0.83%～
Between 4.30%, the RSD of day to day precision controls between 1.53%～3.90%, meets the requirement of quantitative analysis；
(3) detection limit of the C18 fat acid isomer method that the present invention sets up is between 0.009～0.075mg/L, minimum
Determination limit is between 0.028～0.225mg/L；Significantly reduce detection limit and the determination limit of C18 cis-trans-isomer；
(4) linear relationship of the C18 fat acid isomer method that the present invention sets up：The instrumental response value of each cis-trans-isomer
It is in good linear correlation with concentration, linear relationship is above 0.999, fully meets the requirement of quantitative analysis.
In sum, the inventive method is with strong points, pre-treatment is simple to operate, esterifying efficiency is high, method is stable, sensitivity
Height, high specificity, application easy to spread.
Part is embodied by the further advantage of the present invention, target and feature by description below, and part also will be by this
Invention research and practice and be understood by the person skilled in the art.
Part is embodied by the further advantage of the present invention, target and feature by description below, and part also will be by this
Invention research and practice and be understood by the person skilled in the art.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
It should be appreciated that used herein such as " have ", "comprising" and " inclusion " term do not allot one or many
The presence of individual other element or a combination thereof or interpolation.
The present invention provides a kind of gas chromatography of C18 fat acid isomer in detection grease, applies highly polar ion
C18 fat acid isomer in liquid gas phase SLB-IL111 chromatogram post detection grease；Wherein, highly polar ionic liquid gas phase SLB-IL111
The specification of chromatographic column is 200m × 0.25mm × 0.20 μm.
In a preferred version, apply C18 fat in highly polar ionic liquid gas phase SLB-IL111 chromatogram post separation grease
Chromatographic condition during acid isomer is：
Injector temperature：200-230℃；Sample size：1μL；Split ratio：60-100:1；
Chromatographic column initial temperature is 60-80 DEG C, after retaining 5min, is warming up to 175 DEG C with 10-20 DEG C/min, then retains 15-
30min, then it is warming up to 185 DEG C with 1-5 DEG C/min, retain 15-70min；
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
In a preferred version, apply C18 fat in highly polar ionic liquid gas phase SLB-IL111 chromatogram post separation grease
Chromatographic condition during acid isomer is：
Injector temperature：200℃；Sample size：1μL；Split ratio：60:1；
Chromatographic column initial temperature is 60 DEG C, after retaining 5min, is warming up to 175 DEG C with 20 DEG C/min, then retains 15min, then
It is warming up to 185 DEG C with 1 DEG C/min, retain 70min；
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
In a preferred version, also include pre-treatment：
1) weigh 200mg grease to be placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution；
2) add the potassium hydroxide methanol solution of 0.1mL 2-5mol/L, vortex mixes 30s；
3) 10min is centrifuged with 4000rpm, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtain detection sample；
4) detection sample is isolated C18 aliphatic acid therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column different
Structure body.
Preferably, wherein, also include pre-treatment：
1) weigh 200mg grease to be placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution；
2) add the potassium hydroxide methanol solution of 0.1mL 2mol/L, vortex mixes 30s；
3) 10min is centrifuged with 4000rpm, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtain detection sample；
4) detection sample is isolated C18 aliphatic acid therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column different
Structure body.
In a preferred version, the detection limit of C18 fat acid isomer between 0.009～0.075mg/L, survey by minimum
Fixed limit is between 0.028～0.225mg/L.
In a preferred version, described grease is animal oil or vegetable oil.
In a preferred version, the pre-treating method of described animal breast is：
1) weigh 200mg animal breast to be respectively placed in 10mL centrifuge tube, be added thereto to the C11 of 2mL:0 internal standard solution and 3mL
Toluene, adds the chloroacetic chloride methanol solution of 4mL10%, nitrogen charging 1min, and vortex mixes in 80 DEG C of water-bath 2h, every 20min concussion
Once；
2), after taking-up 10mL centrifuge tube is cooled to room temperature, material in 10mL centrifuge tube is transferred in 30mL centrifuge tube I, point
Do not dissolve and wash away 3 times afterwards with the sodium carbonate of 3mL 6%, liquid will be dissolved and washed away and be incorporated in 30mL centrifuge tube II, mix, 5000r/min from
Heart 5min, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtains detection sample；
3) detection sample is isolated C18 aliphatic acid therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column different
Structure body.
In order to better illustrate the accuracy of the C18 aliphatic acid method of separating isomers of foundation, carry out as described below：
The retention time of table 1 C18 cis-trans-isomer and the separating degree at adjacent two peaks
From upper table 1, after applying the inventive method to detect the standard items of C18 cis-trans-isomer, C18:1、C18:2 Hes
C18:Separating degree between 3 regions is respectively 12.723 and 10.349, illustrates that these three regions do not interfere with each other, can divide completely
From.C18:1 and C18:The separating degree of 7 kinds of isomers in 2 regions is both greater than 1.5, illustrates can be kept completely separate between two peaks.C18:
3 have 8 kinds of cis-trans-isomers, completely separable between three transisomers and other isomers, and two kinds of double transisomers
C18:3-9t, 12t, 15c and C18:The appearance time of 3-9t, 12c, 15t is more close, but two peak-to-peak points can distinguish, separating degree
For 0.618, approximate quantitative analysis can be carried out；Also can be kept completely separate between single lens reflex type isomers and other isomers.Above knot
Fruit explanation has been obviously improved C18 using long highly polar ionic liquid chromatographic column SLB-IL111:1 and C18:2 separating degree, and
Achieve C18:The efficiently separating of 3 isomers.
The instrument withinday precision of table 2 C18 cis-trans-isomer and day to day precision
Instrument precision is the common method evaluating chromatogram analysis method to same sample measurement result repeatability, generally uses
Relative standard deviation (RSD) is representing.This experiment adopts same chromatogram analysis method to mix mark solution respectively to C18 along trans-fatty acids
Carry out in a few days (measuring 7 times in one day) and (continuous 7 days mensure) precision is investigated in the daytime. shown.From upper table 2,3 kinds
C18:1 isomers, 4 kinds of C18:2 isomers and 8 kinds of C18:The RSD value of the withinday precision of 3 isomers controls 0.83%～
Between 4.30%, the RSD value of day to day precision controls between 1.53%～3.90%, meets the requirement of quantitative analysis.
The concentration of table 3 cis-trans-isomer and the linear relationship of response
As shown in Table 3, C18:1、C18:2 and C18:The detection limit of 3 each cis-trans-isomers 0.009～0.075mg/L it
Between, minimum determination limit is between 0.028～0.225mg/L.Result also indicates that, under conditions of existing instrument and parameter used,
15 kinds of C18 cis-trans-isomers of 0.08mg/L can qualitative detect, and 15 kinds of C18 cis-trans-isomers of 0.23mg/L can be carried out
Quantitative analysis is it will be apparent that reduce detection limit and the determination limit of C18 cis-trans-isomer.
The concentration of table 4 cis-trans-isomer and the linear relationship of response
15 kinds of C18 fat acid isomer methacrylate calibration solution are carried out gradient dilution, the dilution of each concentration is mixed standard liquid
By set up method carry out gas chromatographic analysis, carry out linear fit in the concentration range investigated, obtain linear equation and
Coefficient correlation (as upper table 4).Result shows that the instrumental response value of each cis-trans-isomer of C18 and concentration are in good linear relationship,
Linear relationship is above 0.999, fully meets the requirement of quantitative analysis.
Embodiment 1 carries out the gas chromatographic analysis of C18 fat acid isomer using the inventive method to vegetable oil.
Pre-treatment：The qualitative and quantitative analysis of C18 isomers in grease：
Weigh 200mg linseed oil, perilla herb oil, soybean oil and corn oil to be respectively placed in 10mL centrifuge tube, add 2mL's
C11:0 internal standard solution, adds the potassium hydroxide methanol solution of 0.1mL 2mol/L, and vortex mixes 30s.With 4000rpm centrifugation
10min.Supernatant 20 μ L is taken to be settled to 1mL volumetric flask, using Shimadzu GC-2010 gas Chromatographic Determination, chromatographic column is SLB-
IL111(200m×0.25mm×0.20μm).
Chromatographic condition, injector temperature：230℃；Sample size：1μL；Split ratio：60:1.
Chromatographic column initial temperature is 60 DEG C, after retaining 5min, is warming up to 175 DEG C with 10 DEG C/min, then retains 15min, then
It is warming up to 185 DEG C with 1 DEG C/min, retain 15min.
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
Carrier gas, High Purity Nitrogen；Inlet pressure：192.2kPa, total flow (Total Flow), 31.5mL/min；Cleaning stream
Amount (Purge Flow), 1.0mL/min
Testing result such as table 5 below：
The concentration of C18 fat acid isomer in table 5 linseed oil, perilla herb oil, soybean oil and corn oil
As shown in Table 5, in linseed oil, perilla herb oil, soybean oil and corn oil, C18 isomers mainly has C18:1-9c、
C18:1-11c、C18:2-9c, 12c and C18:3-9c, 12c, 15c cis-isomer.Wherein perilla herb oil, soybean oil and corn oil
Containing a small amount of trans C18:2-9t, 12t isomers；A small amount of trans C18 is contained in soybean oil:2-9c, 12t and C18:2-
9t, 12c isomers；No trans C18 in corn oil:3-9c, 12c, 15t isomers, illustrates that the method set up can be effectively qualitative
C18 fatty acid composition in quantitative analysis vegetable oil and fatty foods.
Embodiment 2 carries out the gas chromatographic analysis of C18 fat acid isomer using the inventive method to animal oil.
Pre-treatment：The qualitative and quantitative analysis of C18 isomers in grease：
Weigh 200mg animal oil to be respectively placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution, adds 0.1mL
The potassium hydroxide methanol solution of 3.5mol/L, vortex mixes 30s.10min is centrifuged with 4000rpm.Supernatant 20 μ L is taken to be settled to
1mL volumetric flask, using Shimadzu GC-2010 gas Chromatographic Determination, chromatographic column is SLB-IL111 (200m × 0.25mm × 0.20 μ
m).
Chromatographic condition, injector temperature：200℃；Sample size：1μL；Split ratio：80:1.
Chromatographic column initial temperature is 70 DEG C, after retaining 5min, is warming up to 175 DEG C with 15 DEG C/min, then retains 22min, then
It is warming up to 185 DEG C with 3 DEG C/min, retain 35min.
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
Testing result such as table 6 below：
The concentration of C18 fat acid isomer in table 6 animal oil：
As shown in Table 6, in lard, C18 isomers has C18:1-9c、C18:1-11c、C18:2-9c, 12c and C18:3-9c,
12c, 15c isomers, wherein C18:The content highest of 1-9c, and C18:The content of 3-9c, 12c, 15c is minimum.C18 in lard
Isomers is all cis, no transisomer, also confirms that the method for foundation is adapted in qualitative, quantitative transfer thing fatty foods
C18 fatty acid composition.
Embodiment 3 carries out the gas chromatographic analysis of C18 fat acid isomer using the inventive method to animal breast.
Pre-treatment：The qualitative and quantitative analysis of C18 isomers in animal breast：
Weigh 200mg milk to be respectively placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution and 3mL toluene, then plus
Enter the chloroacetic chloride methanol solution of 4mL10%, nitrogen charging 1min, vortex mixes in 80 DEG C of water-bath 2h, and every 20min shakes once, takes out
It is transferred to after being cooled to room temperature in 30mL centrifuge tube, is washed 3 times with the sodium carbonate liquor of 3mL 6% respectively, be incorporated into 30mL centrifugation
Guan Zhong, mixes, and 5000r/min is centrifuged 5min, takes supernatant, and using Shimadzu GC-2010 gas Chromatographic Determination, chromatographic column is SLB-
IL111(200m×0.25mm×0.20μm).
Chromatographic condition, injector temperature：230℃；Sample size：1μL；Split ratio：100:1.
Chromatographic column initial temperature is 60 DEG C, after retaining 5min, is warming up to 175 DEG C with 20 DEG C/min, then retains 15min, then
It is warming up to 185 DEG C with 5 DEG C/min, retain 70min.
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
Carrier gas, High Purity Nitrogen；Inlet pressure：192.2kPa, total flow (Total Flow), 31.5mL/min；Cleaning stream
Amount (Purge Flow), 1.0mL/min.
Testing result such as table 7 below：
The concentration of C18 fat acid isomer in table 7 animal breast：
As shown in Table 7, in animal breast, C18 isomers has 8 kinds, predominantly cis C18:1-9c isomers, also contains a small amount of
C18:1-9t、C18:2-9c, 12t and C18:2-9t, 12t isomers, illustrates that the gas chromatography set up is also adapted to fixed
Property quantitative analysis animal breast in C18 fatty acid composition.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and embodiment
With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily
Realize other modification, therefore under the universal being limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details with shown here as the embodiment with description.
Claims (8)
1. a kind of gas chromatography detecting C18 fat acid isomer in grease is it is characterised in that apply highly polar ionic liquid
C18 fat acid isomer in gas phase SLB-IL111 chromatogram post detection grease；Wherein, highly polar ionic liquid gas phase SLB-IL111 color
The specification of spectrum post is 200m × 0.25mm × 0.20 μm.
2. the gas chromatography detecting C18 fat acid isomer in grease as claimed in claim 1 is it is characterised in that answer
With chromatographic condition during C18 fat acid isomer in highly polar ionic liquid gas phase SLB-IL111 chromatogram post separation grease it is：
Injector temperature：200-230℃；Sample size：1μL；Split ratio：60-100:1；
Chromatographic column initial temperature is 60-80 DEG C, after retaining 5min, is warming up to 175 DEG C with 10-20 DEG C/min, then retains 15-
30min, then it is warming up to 185 DEG C with 1-5 DEG C/min, retain 15-70min；
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
3. the gas chromatography detecting C18 fat acid isomer in grease as claimed in claim 1 is it is characterised in that answer
With chromatographic condition during C18 fat acid isomer in highly polar ionic liquid gas phase SLB-IL111 chromatogram post separation grease it is：
Injector temperature：230℃；Sample size：1μL；Split ratio：60:1；
Chromatographic column initial temperature is 60 DEG C, after retaining 5min, is warming up to 175 DEG C with 20 DEG C/min, then retains 15min, then with 1
DEG C/min is warming up to 185 DEG C, retains 70min；
Detector：Flame ionization ditector (FID)；Detector temperature：250℃；Tail wind drift amount, 30.0mL/min；
Hydrogen flowing quantity 40mL/min；Air mass flow, 400mL/min.
4. the gas chromatography detecting C18 fat acid isomer in grease as claimed in claim 1 is it is characterised in that go back
Including pre-treatment：
1) weigh 200mg grease to be placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution；
2) add the potassium hydroxide methanol solution of 0.1mL 2-5mol/L, vortex mixes 30s；
3) 10min is centrifuged with 4000rpm, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtain detection sample；
4) detection sample is isolated C18 fat acid isomer therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column.
5. the gas chromatography detecting C18 fat acid isomer in grease as claimed in claim 1 is it is characterised in that go back
Including pre-treatment：
1) weigh 200mg grease to be placed in 10mL centrifuge tube, add the C11 of 2mL:0 internal standard solution；
2) add the potassium hydroxide methanol solution of 0.1mL 2mol/L, vortex mixes 30s；
3) 10min is centrifuged with 4000rpm, takes supernatant 20 μ L to be settled to 1mL volumetric flask, obtain detection sample；
4) detection sample is isolated C18 fat acid isomer therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column.
6. in detection grease as claimed in claim 1 the gas chromatography of C18 fat acid isomer it is characterised in that C18
, between 0.009～0.075mg/L, minimum determination limit is between 0.028～0.225mg/L for the detection limit of fatty acid isomer.
7. the gas chromatography detecting C18 fat acid isomer in grease as any one of claim 1-6, it is special
Levy and be, described grease is animal oil or vegetable oil.
8. the gas chromatography detecting C18 fat acid isomer in grease as any one of claim 1-3, it is special
Levy and be, described grease is animal breast, the pre-treating method of described animal breast is：
1) weigh 200mg animal breast to be respectively placed in 10mL centrifuge tube, be added thereto to the C11 of 2mL:0 internal standard solution and 3mL first
Benzene, adds the chloroacetic chloride methanol solution of 4mL10%, nitrogen charging 1min, and vortex mixes in 80 DEG C of water-bath 2h, every 20min concussion one
Secondary；
2), after taking-up 10mL centrifuge tube is cooled to room temperature, material in 10mL centrifuge tube is transferred in 30mL centrifuge tube I, uses respectively
The sodium carbonate liquor of 3mL6% washes 3 times afterwards, is incorporated in 30mL centrifuge tube II, mixes, and 5000r/min is centrifuged 5min, takes
Clear liquid 20 μ L is settled to 1mL volumetric flask, obtains detection sample；
3) detection sample is isolated C18 fat acid isomer therein through highly polar ionic liquid gas phase SLB-IL111 chromatographic column.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113311098A (en) * | 2021-05-21 | 2021-08-27 | 汤臣倍健股份有限公司 | Method for measuring content of free fatty acid in breast milk |
| TWI823798B (en) * | 2023-03-13 | 2023-11-21 | 高雄醫學大學 | Kit and method for detecting trans fatty acid |
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2016
- 2016-09-26 CN CN201610853228.4A patent/CN106442824B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113311098A (en) * | 2021-05-21 | 2021-08-27 | 汤臣倍健股份有限公司 | Method for measuring content of free fatty acid in breast milk |
| CN113311098B (en) * | 2021-05-21 | 2022-07-29 | 汤臣倍健股份有限公司 | Method for measuring content of free fatty acid in breast milk |
| TWI823798B (en) * | 2023-03-13 | 2023-11-21 | 高雄醫學大學 | Kit and method for detecting trans fatty acid |
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