CN103149303B - The rapid assay methods of fatty acid and squalene in vegetable oil - Google Patents
The rapid assay methods of fatty acid and squalene in vegetable oil Download PDFInfo
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- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 41
- 239000000194 fatty acid Substances 0.000 title claims abstract description 41
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 41
- 150000004665 fatty acids Chemical class 0.000 title claims abstract description 41
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 title claims abstract description 38
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 title claims abstract description 38
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229940031439 squalene Drugs 0.000 title claims abstract description 38
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000003556 assay Methods 0.000 title claims abstract description 12
- 235000015112 vegetable and seed oil Nutrition 0.000 title abstract description 19
- 239000008158 vegetable oil Substances 0.000 title abstract description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 15
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- 238000004587 chromatography analysis Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000010606 normalization Methods 0.000 claims abstract description 8
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 12
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 12
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 7
- 238000004817 gas chromatography Methods 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 239000010453 quartz Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001228 spectrum Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- BITHHVVYSMSWAG-KTKRTIGZSA-N (11Z)-icos-11-enoic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCC(O)=O BITHHVVYSMSWAG-KTKRTIGZSA-N 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- ZVRMGCSSSYZGSM-CCEZHUSRSA-N (E)-hexadec-2-enoic acid Chemical compound CCCCCCCCCCCCC\C=C\C(O)=O ZVRMGCSSSYZGSM-CCEZHUSRSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- 235000021314 Palmitic acid Nutrition 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229940108623 eicosenoic acid Drugs 0.000 claims description 6
- BITHHVVYSMSWAG-UHFFFAOYSA-N eicosenoic acid Natural products CCCCCCCCC=CCCCCCCCCCC(O)=O BITHHVVYSMSWAG-UHFFFAOYSA-N 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- 235000020778 linoleic acid Nutrition 0.000 claims description 6
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 claims description 6
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 239000008117 stearic acid Substances 0.000 claims description 6
- 230000032050 esterification Effects 0.000 abstract description 7
- 238000005886 esterification reaction Methods 0.000 abstract description 7
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 2
- 230000001627 detrimental effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000000419 plant extract Substances 0.000 description 2
- 239000010773 plant oil Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000005477 standard model Effects 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
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Abstract
The invention provides the rapid assay methods of fatty acid and squalene in a vegetable oil, by the amount of 35 ~ 50mL/g vegetable oil, normal hexane is added in vegetable oil, vegetable oil is dissolved completely, again by the amount of 5.5 ~ 7.5mL/g vegetable oil, adding concentration is the potassium hydroxide of 2mol/L and the mixed solution of methyl alcohol, vibration 3 ~ 5min, centrifuging 5 ~ 8min, obtains upper sample liquid; Supply gas and carry out GC, MS in chromatography and analyze, and calculate the percentage composition of each fatty acid composition and functional components squalene routinely by area normalization method.The extraction of sample fatty acid and the esterification of fatty acid synchronously complete, and squalene is extracted well in solvent simultaneously, and quick, simple and direct, quantity of solvent is little, is not detrimental to health, and achieves lower detection limit.Be applicable to the detection of fatty acid and squalene content in any vegetable oil.
Description
Technical field
The present invention relates to a kind of plant component assay method, in especially a kind of olive oil, the rapid assay methods of fatty acid and squalene, belongs to technical field of analytical chemistry.
Technical background
In plant extract, plant component are analyzed, usually relate to the mensuration of main fatty acid and functional components in vegetable oil.Existing technical standard is all with loaded down with trivial details, complicated operation, and need multiple toxic reagent (as the concentrated sulphuric acid, sherwood oil, benzene, ether etc.) the esterification method that coordinates, the early stage of carrying out olive oil processes, because treatment effect is undesirable, when the olive oil processed is sent in gas chromatograph analyze time, chromatographic peak can be caused not occur, or the separating effect of fatty acid and squalene two principal ingredient is undesirable, and main fatty acid component in separation olive oil and functional components time, the two capillary posts also needing polarity different, namely fatty acid analysis will use polar column, the analysis of functional components squalene is then with non-polar column, and fatty acid is also different from the earlier stage processing method of squalene in separation olive oil, namely be separated two kinds of compositions and need two kinds of esterification methods.Because of but cause that plant extract analysis cost remains high, the main cause of precision of analysis deficiency all the time.Therefore, be necessary to be improved prior art completely.
Summary of the invention
For overcoming in prior art, loaded down with trivial details, complex operations that Plant Oil Fatty Acid Methyl Ester method exists, time-consuming, effort, and harmful, toxic reagent to be used, the deficiencies such as cost is high, serious waste of resources, the invention provides a kind of convenient, fast, cost is low, and sample only needs once process in early stage, can realize the method for separating and assaying of main fatty acid and functional components squalene in vegetable oil with same root chromatogram column.
The present invention is realized by following technical proposal: the rapid assay methods of fatty acid and squalene in a vegetable oil, is characterized in that through the following step:
A, amount by 35 ~ 50mL/g vegetable oil, add normal hexane, vegetable oil dissolved completely in vegetable oil, again by the amount of 5.5 ~ 7.5mL/g vegetable oil, adding concentration is the potassium hydroxide of 2mol/L and the mixed solution of methyl alcohol, vibration 3 ~ 5min, centrifuging 5 ~ 8min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and calculate the percentage composition of each fatty acid composition and functional components squalene routinely by area normalization method, wherein:
GC analysis condition: a HP-5MS quartz capillary column; Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
Described normal hexane, potassium hydroxide and methyl alcohol are commercial chromatographic grade product.
The gas chromatograph model of described step B is HP6890GC/5973MS gas chromatography-GC-MS.
The present invention has following advantages and effect: when adopting such scheme to measure main fatty acid and squalene in vegetable oil, its esterification method is quick, simple and direct, and the quantity of solvent used is little, to health without any harm, be easy to recycle, greatly solvent cost can be reduced during batch production, the shortening time, reduce unnecessary waste, economize on resources, when using the method simultaneously, the extraction of sample fatty acid and the esterification of fatty acid synchronously complete, squalene is extracted well in solvent simultaneously, selected nonpolar capillary column squalene in same heating schedule is good with being separated of each fatty acid methyl ester, quantitatively accurately, and achieve lower detection limit.Use GC-MS and squalene standard model method to measure the content of squalene in olive oil, the preci-sion and accuracy of its method is good, can reach required testing goal, and this method is also applicable to the detection of fatty acid and squalene content in other vegetable oil.
Accompanying drawing explanation
Fig. 1 is olive oil gas chromatogram of the present invention.
Known in Fig. 1, the inventive method only needs 35min just can complete being separated of main fatty acid component and functional components squalene in vegetable oil simultaneously, good separation, conventional method then needs more than the 3 times times (three times of times of 35min) could realize being separated of main fatty acid and functional components in vegetable oil, does not wherein also comprise changing pillar and equilibration time also has time for sample pretreatment; The esterification time only needs 15min, and the methyl esterification of fatty acid time of conventional method about needs 60 ~ 90min; The analysis of a plant oil sample only needs 50 ~ 60min, and conventional method then needs 100 ~ 130min, and two kinds of compositions then need 200 ~ 260min.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
A rapid assay methods for fatty acid and squalene in olive oil, is characterized in that through the following step:
A, amount by 35mL/g olive oil, add normal hexane 2ml, olive oil dissolved completely in 40mg olive oil, press the amount of 5.5mL/g olive oil again, add the mixed solution 0.3mL of potassium hydroxide that concentration is 2mol/L and methyl alcohol, vibration 3min, centrifuging 5min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and the percentage composition of each fatty acid composition and functional components squalene in olive oil is calculated routinely by area normalization method, be respectively: total fatty acid content 94.10% (respectively: gaidic acid 1.05%, palmitic acid 14.14%, linoleic acid 16.01%, oleic acid 60.44%, stearic acid 1.50%, eicosenoic acid 0.29%, arachidic acid 0.30%, unknown 0.20%, mountain Yu's acid 0.17%); Squalene content 5.90%.
Wherein:
GC analysis condition: a HP-5MS quartz capillary column (30m × 0.32mm × 0.25 μm); Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
Embodiment 2
A rapid assay methods for fatty acid and squalene in olive oil, is characterized in that through the following step:
A, amount by 40mL/g olive oil, add normal hexane 2mL, olive oil dissolved completely in 50mg olive oil, press the amount of 6mL/g olive oil again, add the mixed solution 0.3mL of potassium hydroxide that concentration is 2mol/L and methyl alcohol, vibration 4min, centrifuging 6min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and the percentage composition of each fatty acid composition and functional components squalene in olive oil is calculated routinely by area normalization method, be respectively: content of fatty acid 91.70% (respectively: gaidic acid 1.36%, palmitic acid 15.18%, linoleic acid 10.14%, oleic acid 62.33%, stearic acid 1.58%, eicosenoic acid 0.31%, arachidic acid 0.33%, unknown 0.17%, mountain Yu's acid 0.30%); Squalene content 8.30%.
Wherein:
GC analysis condition: a HP-5MS quartz capillary column (30m × 0.32mm × 0.25 μm); Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
Embodiment 3
A rapid assay methods for fatty acid and squalene in olive oil, is characterized in that through the following step:
A, amount by 50mL/g olive oil, add normal hexane 2mL, olive oil dissolved completely in 60mg olive oil, press the amount of 7.5mL/g olive oil again, add the mixed solution 0.3mL of potassium hydroxide that concentration is 2mol/L and methyl alcohol, vibration 5min, centrifuging 8min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and the percentage composition of each fatty acid composition and functional components squalene in olive oil is calculated routinely by area normalization method, be respectively: content of fatty acid 95.97% (respectively: gaidic acid 1.07%, palmitic acid 14.10%, linoleic acid 8.01%, oleic acid 69.99%, stearic acid 1.60%, eicosenoic acid 0.24%, arachidic acid 0.32%, unknown 0.24%, mountain Yu's acid 0.40%); Squalene content 4.03%.
Wherein:
GC analysis condition: a HP-5MS quartz capillary column (30m × 0.32mm × 0.25 μm); Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
Claims (3)
1. the rapid assay methods of fatty acid and squalene in olive oil, is characterized in that through the following step:
A, amount by 35mL/g olive oil, add normal hexane 2ml, olive oil dissolved completely in 40mg olive oil, press the amount of 5.5mL/g olive oil again, add the mixed solution 0.3mL of potassium hydroxide that concentration is 2mol/L and methyl alcohol, vibration 3min, centrifuging 5min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and the percentage composition of each fatty acid composition and functional components squalene in olive oil is calculated routinely by area normalization method, be respectively: total fatty acid content 94.10%, wherein: gaidic acid 1.05%, palmitic acid 14.14%, linoleic acid 16.01%, oleic acid 60.44%, stearic acid 1.50%, eicosenoic acid 0.29%, arachidic acid 0.30%, unknown 0.20%, mountain Yu's acid 0.17%; Squalene content 5.90%, wherein:
GC analysis condition: the HP-5MS quartz capillary column of 30m × 0.32mm × 0.25 μm; Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
2. the rapid assay methods of fatty acid and squalene in olive oil, is characterized in that through the following step:
A, amount by 40mL/g olive oil, add normal hexane 2mL, olive oil dissolved completely in 50mg olive oil, press the amount of 6mL/g olive oil again, add the mixed solution 0.3mL of potassium hydroxide that concentration is 2mol/L and methyl alcohol, vibration 4min, centrifuging 6min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and the percentage composition of each fatty acid composition and functional components squalene in olive oil is calculated routinely by area normalization method, be respectively: content of fatty acid 91.70%, wherein: gaidic acid 1.36%, palmitic acid 15.18%, linoleic acid 10.14%, oleic acid 62.33%, stearic acid 1.58%, eicosenoic acid 0.31%, arachidic acid 0.33%, unknown 0.17%, mountain Yu's acid 0.30%; Squalene content 8.30%, wherein:
GC analysis condition: the HP-5MS quartz capillary column of 30m × 0.32mm × 0.25 μm; Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
3. the rapid assay methods of fatty acid and squalene in olive oil, is characterized in that through the following step:
A, amount by 50mL/g olive oil, add normal hexane 2mL, olive oil dissolved completely in 60mg olive oil, press the amount of 7.5mL/g olive oil again, add the mixed solution 0.3mL of potassium hydroxide that concentration is 2mol/L and methyl alcohol, vibration 5min, centrifuging 8min, obtains upper sample liquid;
Carry out GC, MS in B, chromatography of being supplied gas by steps A gained test liquid to analyze, and the percentage composition of each fatty acid composition and functional components squalene in olive oil is calculated routinely by area normalization method, be respectively: content of fatty acid 95.97%, wherein: gaidic acid 1.07%, palmitic acid 14.10%, linoleic acid 8.01%, oleic acid 69.99%, stearic acid 1.60%, eicosenoic acid 0.24%, arachidic acid 0.32%, unknown 0.24%, mountain Yu's acid 0.40%; Squalene content 4.03%, wherein:
GC analysis condition: the HP-5MS quartz capillary column of 30m × 0.32mm × 0.25 μm; Temperature programme: be warming up to 300 DEG C by the heating rate of 3 DEG C/min; Injector temperature 290 DEG C; Post flow 1.0mL/min; Pressure 100kPa before post; Sample size 0.5 ~ 1.0 μ L; Split ratio 10: 1; Carrier gas is high-purity helium;
MS analysis condition: ionization mode EI; Electron energy 70; Transmission line temperature 250 DEG C; Ion source temperature 230 DEG C; Quadrupole rod temperature 150 DEG C; Mass range 35 ~ 500; Wiley7n.1 standard spectrum storehouse is adopted to carry out retrieval qualitative.
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| CN105784906B (en) * | 2016-04-07 | 2018-03-16 | 浙江大学 | Squalene differentiates the method for building up of label as olive oil and camellia seed oil |
| WO2017173638A1 (en) * | 2016-04-07 | 2017-10-12 | 浙江大学 | Method for using squalene as identification marker of olive oil and camellia seed oil |
| CN106872607A (en) * | 2017-03-17 | 2017-06-20 | 广州康琪莱生物科技有限公司 | A kind of method that high-resolution determines trans-fatty acid in ganoderma lucidum spore oil |
| CN107389847B (en) * | 2017-06-05 | 2020-01-07 | 中国农业科学院蜜蜂研究所 | Method for rapidly analyzing lipid components in bee pollen |
| CN108663453B (en) * | 2018-05-28 | 2021-02-23 | 贵州茅台酒股份有限公司 | Method for determining content of squalene in sorghum |
| CN109001306A (en) * | 2018-06-01 | 2018-12-14 | 南昌大学 | The prediction technique of squalene and sterol index in a kind of tea oil |
| CN110031558A (en) * | 2019-04-11 | 2019-07-19 | 山东省食品药品检验研究院 | The rapid detection method of Fatty Acids from Vegetable Oil and squalene |
| CN113588854A (en) * | 2020-12-21 | 2021-11-02 | 四川国为制药有限公司 | Method for detecting fatty acid composition |
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