CN104931482A - Detection method for oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum - Google Patents
Detection method for oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum Download PDFInfo
- Publication number
- CN104931482A CN104931482A CN201510372342.0A CN201510372342A CN104931482A CN 104931482 A CN104931482 A CN 104931482A CN 201510372342 A CN201510372342 A CN 201510372342A CN 104931482 A CN104931482 A CN 104931482A
- Authority
- CN
- China
- Prior art keywords
- ganoderma lucidum
- raman
- lucidum spore
- spore oil
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 240000008397 Ganoderma lucidum Species 0.000 title claims abstract description 124
- 235000001637 Ganoderma lucidum Nutrition 0.000 title claims abstract description 123
- 238000001514 detection method Methods 0.000 title claims abstract description 40
- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 26
- 230000003647 oxidation Effects 0.000 title abstract description 5
- 238000007254 oxidation reaction Methods 0.000 title abstract description 5
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 92
- 239000002253 acid Substances 0.000 claims abstract description 58
- 150000002978 peroxides Chemical class 0.000 claims abstract description 54
- 238000011156 evaluation Methods 0.000 claims abstract description 29
- 238000012360 testing method Methods 0.000 claims abstract description 19
- 230000001590 oxidative effect Effects 0.000 claims description 41
- 238000004448 titration Methods 0.000 claims description 27
- 238000013507 mapping Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 8
- 238000012937 correction Methods 0.000 claims description 7
- 230000003071 parasitic effect Effects 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 27
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000003921 oil Substances 0.000 description 115
- 239000000523 sample Substances 0.000 description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 43
- 239000003963 antioxidant agent Substances 0.000 description 20
- 235000006708 antioxidants Nutrition 0.000 description 20
- 230000003078 antioxidant effect Effects 0.000 description 19
- 235000011121 sodium hydroxide Nutrition 0.000 description 15
- 239000007788 liquid Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 9
- 235000019345 sodium thiosulphate Nutrition 0.000 description 9
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 8
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 5
- 229930003427 Vitamin E Natural products 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 4
- 238000012067 mathematical method Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 150000008442 polyphenolic compounds Chemical class 0.000 description 4
- 235000013824 polyphenols Nutrition 0.000 description 4
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 4
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 4
- 235000019165 vitamin E Nutrition 0.000 description 4
- 229940046009 vitamin E Drugs 0.000 description 4
- 239000011709 vitamin E Substances 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 241000222336 Ganoderma Species 0.000 description 3
- 238000002479 acid--base titration Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 230000036962 time dependent Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 244000000231 Sesamum indicum Species 0.000 description 2
- 235000003434 Sesamum indicum Nutrition 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000008034 disappearance Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000002095 near-infrared Raman spectroscopy Methods 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 210000004881 tumor cell Anatomy 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 235000007466 Corylus avellana Nutrition 0.000 description 1
- 240000003211 Corylus maxima Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- RDMQPKIDHAFXKA-JNORPAGFSA-N Ganoderic Acid Am1 Chemical compound C([C@@]12C)C[C@H](O)C(C)(C)[C@@H]1CC(=O)C1=C2C(=O)C[C@]2(C)[C@@H]([C@@H](CC(=O)CC(C)C(O)=O)C)CC(=O)[C@]21C RDMQPKIDHAFXKA-JNORPAGFSA-N 0.000 description 1
- 229930182735 Ganoderic acid Natural products 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000222341 Polyporaceae Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000036436 anti-hiv Effects 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000007969 cellular immunity Effects 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000001261 hydroxy acids Chemical class 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 239000002777 nucleoside Substances 0.000 description 1
- 125000003835 nucleoside group Chemical group 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 210000005132 reproductive cell Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000011506 response to oxidative stress Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 210000000813 small intestine Anatomy 0.000 description 1
- 210000000130 stem cell Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention provides a detection method of oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum, wherein the oxidation rancidity degree of the ganoderma lucidum spore oil takes the acid value and the peroxide value of the ganoderma lucidum spore oil as evaluation indexes, and the detection method comprises the following steps: firstly, 1655cm in Raman spectrogram of standard sample-1The integral intensity of the Raman peak is plotted by a vertical coordinate and the acid value or the peroxide value is plotted by a horizontal coordinate, and an evaluation standard chart of the acid value and the peroxide value of the ganoderma lucidum spore oil is established; then, the Raman spectrum of the test sample was measured and 1655cm was obtained-1Comparing the Raman peak integral intensity result with an acid value and peroxide value evaluation standard chart respectively to obtain an acid value and a peroxide value of the sample to be tested, and further obtaining an oxidation rancidity degree evaluation result of the ganoderma lucidum spore oil sample to be tested; the method has the advantages of short detection time, low sample consumption, simple and convenient operation and capability of realizing on-site quick detection, so that the detection method has a great practical application prospect.
Description
(1) technical field
The present invention relates to a kind of detection method of ganoderma lucidum spore oil oxidative rancidity, be specifically related to a kind of method of the quick detection ganoderma lucidum spore oil oxidative rancidity degree based on Raman spectrum.
(2) background technology
Glossy ganoderma, also known as polyporus lucidus, is the complete stool of the red sesame of Polyporaceae plant or purple sesame, is just praised highly as Chinese medicine is top grade since ancient times, just early on the books at traditional Chinese medicine ancient books and records such as Shennong's Herbals.Reishi sporule is the sexual reproductive cell of glossy ganoderma, general in filbert to tawny, avette, and size generally, between (long × wide) (8.5 ~ 11.2) μm × (5.2 ~ 6.9) μm, includes ganoderma lucidum spore oil.Ganoderma lucidum spore oil has concentrated the elite of effective component of glossy ganoderma, is rich in triterpenes ganoderic acid, ganoderan, nucleosides, amino acid, saturated with various active compositions such as unsaturated fatty acid, organic germanium and other trace elements.Numerous research shows, ganoderma lucidum spore oil has functions such as strengthening cellular immunity, enhancing NK cytoactive, reducing blood lipid, immunological regulation, but directly can kill tumor stem cell, the apoptosis of inhibition tumor cell propagation and induced tumor cell, anti-oxidant and alleviate bladder blocking, and the function of anti-HIV activity.Simultaneously because its unsaturated fatty acid content is very high, have more the effect improving cardiovascular and cerebrovascular disease, anti arteriosclerosis, reducing blood lipid, norcholesterol.
Because ganoderma lucidum spore oil effect is remarkable, expensive, therefore on market, Related product quality is uneven, has a strong impact on consumer's interests.Ganoderma lucidum spore oil is rich in unsaturated double-bond, spore oil is in storage, transportation, especially be very easily oxidized under the condition of high temperature, high humidity, main generation is attacked double bond by active oxygen radical and is caused degraded, produce detrimental oxide, the superoxide such as multiple aldehyde, ketone, alcohol, acid and hydroxy acid, generate strong impulse smell (oxidative rancidity) the normal biochemical functions of body can be destroyed (as cause body response to oxidative stress, reduce body's immunity, cause the organ such as small intestine, liver loose), severe damaging body health.
At present, usually adopt in the industry the quality monitoring index of edible oil and peroxide value, acid number as the prevailing quality monitor control index of spore oil.And the method mainly titrimetry of domestic mensuration ganoderma lucidum spore oil acid number, peroxide value, comprise standard acid-base titrimetric and redox titration, but how much there is following defect in titrimetry: as trivial operations, need professional to analyze in laboratory; Length consuming time, detects and needs a few hours to complete; Not portable, be difficult to outdoor Site Detection; Insufficient sensitivity is high, and consume sample size many (5 ~ 10g), testing cost is high.
In recent years along with the development of modernization detection technique, some new technologies are constantly used to field of food detection, as HPLC, NMR, application of gas chromatorgraphy/mass (GC-MS), fluorescence spectrum etc.These methods have certain advantage compared with classic method, but when detecting, especially to this kind of material costly of ganoderma lucidum spore oil, all have certain limitation.As high performance liquid chromatography (HPLC), with classic method ratio, have at a high speed, sample is destroyed, the easy advantage such as recoverys, but it is not portable, is difficult to outdoor detection, compared with Raman spectrum, its sensitivity is still not so good as Raman spectrum, consuming time also longer.When chromatography (GC) detects, although its discrimination efficiency is high, quantitative test is easy, and its qualitative ability is poor.And mass spectroscopy (MS), corresponding with chromatography, its qualitative ability is comparatively strong, highly sensitive, but in testing process, require that sample introduction is pure, carries out quantitative test comparatively complicated.
(3) summary of the invention
The object of the invention is to utilize Raman spectroscopy to set up the New Technique for Fast of a kind of dynamic monitoring method of ganoderma lucidum spore oil oxidative rancidity and ganoderma lucidum spore oil acid number, peroxide value, and utilize the method to measure the kinetic parameter of ganoderma lucidum spore oil oxidative rancidity, filter out efficient Reishi sporule oil antioxidant.
For reaching goal of the invention, the technical solution used in the present invention is:
A kind of detection method of the ganoderma lucidum spore oil oxidative rancidity based on Raman spectrum, the oxidative rancidity degree of described ganoderma lucidum spore oil is using the acid number of ganoderma lucidum spore oil (AV), peroxide value (POV) as evaluation index, the oxidative rancidity degree of ganoderma lucidum spore oil increases along with the rising of acid number, peroxide value, and described detection method comprises the steps:
(1) ganoderma lucidum spore oil acid number, peroxide value evaluation criterion figure is set up
Get ganoderma lucidum spore oil, be placed in 70 DEG C of uncovered preservations of thermostat lucifuge, stir every 24 ~ 36h and once mix, in 5 days, sample with the time gradient every 24 hours, after every sub-sampling, sample is detected, measure acid number, the peroxide value of Reishi sporule oil samples by standardized titration method respectively, record the Raman spectrogram of Reishi sporule oil samples with Raman spectrometer, obtain acid number, peroxide value, the Raman spectrogram of series of samples;
The detection method of the Raman spectrum of described ganoderma lucidum spore oil is: get 20 ~ 200 μ L Reishi sporule oil samples, be placed in kapillary or sample hose, put into Raman spectrometer sample cell, laser intensity is selected high-grade, laser irradiation time is set as 10s, automatically carries out the calibration of environment parasitic light and baseline correction, and sample determination is averaged for 5 times times, obtain the Raman spectrogram of Reishi sporule oil samples, 1655cm in calculated Raman spectrum figure
-1raman peaks integrated intensity (Raman peaks integrated intensity calculates with the integrating function of the peak area in analysis software Grams, and software calculates automatically, then copy or export data);
With 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the acid number of sample is horizontal ordinate mapping, obtains the acid number evaluation criterion figure of ganoderma lucidum spore oil; With 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the peroxide value of sample is horizontal ordinate mapping, obtains the peroxide value evaluation criterion figure of ganoderma lucidum spore oil;
(2) detection of test sample
Get 20 ~ 200 μ L ganoderma lucidum spore oil test samples, be placed in kapillary or sample hose, put into Raman spectrometer sample cell, laser intensity is selected high-grade, laser irradiation time is set as 10s, automatically carry out the calibration of environment parasitic light and baseline correction, sample determination is averaged for 5 times, obtains the Raman spectrogram of ganoderma lucidum spore oil test sample; 1655cm in calculated Raman spectrum figure
-1raman peaks integrated intensity, by the 1655cm calculated
-1acid number evaluation criterion figure, peroxide value evaluation criterion figure that Raman peaks integrated intensity result obtains with step (1) respectively contrast, obtain acid number and the peroxide value of test sample, and then draw the oxidative rancidity degree evaluation result of ganoderma lucidum spore oil test sample.
The detection method of the ganoderma lucidum spore oil oxidative rancidity based on Raman spectrum of the present invention, in step (1), the acid number of described Reishi sporule oil samples, the standardized titration method of peroxide value are recorded in: Chinese Pharmacopoeia Commission. Pharmacopoeia of People's Republic of China (). and Beijing: China Medical Science Press, 2010. annex 54-55. and annex 56-57.
Be specially:
The detection of (a) Reishi sporule oil samples acid number
Ganoderma lucidum spore oil acid number is surveyed: in 250mL conical flask, add ethanol, each 25.0mL mixing of ether in advance, accurately take Reishi sporule oil samples 0.500g and add in conical flask, vibration makes it dissolve completely by NaOH standardized titration method.Be titrated to pink with sodium hydroxide titration liquid (0.1mol/L) and continuously 30s is colour-fast, read and consume sodium hydroxide titration liquid long-pending (mL).
The computing formula of acid number:
AV＝(A×5.61)/W (1)
In formula: AV is acid number; A is for consuming the volume (mL) of sodium hydroxide titration liquid (0.1mol/L); W is sample sampling amount (g); 5.61 is the milligram number that every milliliter of sodium hydroxide titration liquid (0.1mol/L) is equivalent to NaOH, can correct according to the actual concentrations demarcating rear sodium hydroxide titration liquid.
The potpourri preparation of ether and ethanol: get ethanol, each 25.0mL of ether in the mixing of 250mL conical flask, first add the instructions phenolphthalein solution 1mL of 0.5% before use, shake up, drip sodium hydroxide titration liquid appropriate, be adjusted to micro-aobvious pink.
The preparation of 0.1mol/L sodium hydroxide titration liquid: first prepare NaOH saturated solution, taking excessive sodium hydrate solid is dissolved in distilled water, wherein sodium hydrate solid solubleness is 111g (20 DEG C), transfer pipet accurately pipette supernatant 1.4mL in 250mL volumetric flask with newly to boil cooling without carbon dioxide distilled water constant volume.
The demarcation of sodium hydroxide titration liquid: accurately take the benchmark Potassium Hydrogen Phthalate being dried to constant weight at 105 DEG C and be about 0.600g, adds the cold water 50.0mL jolting of newly boiling, and makes it dissolve as far as possible; Add 0.5% instructions phenolphthalein solution 2, be titrated to the aobvious pink of solution with this liquid.The sodium hydroxide titration liquid (0.1mol/L) of every 1mL is equivalent to the Potassium Hydrogen Phthalate of 20.42mg.The computing formula of calibration result is:
In formula: W is the sample weighting amount (g) of Potassium Hydrogen Phthalate; V is the volume (mL) that timing signal consumes sodium hydroxide titration liquid.
The preparation of 0.5% phenolphthalein solution: take 0.50g phenolphthalein, is dissolved in the ethanol of 100mL95%, without the need to adding water.Test in triplicate and calculate its mean value.
The detection of (b) Reishi sporule oil samples peroxide value
In the dry iodine flask of 250mL, adding the ganoderma lucidum spore oil of 1.500g, be mixed into the mixed liquor 30.0mL of the chloroform-glacial acetic acid of 1:1 modulation afterwards, shaking up sample by constantly shaking.After fully shaking up, add the saturated solution of potassium iodide that about 1.0mL newly prepares, after adding, shake time half a minute gently, after shaking up, be positioned over dark place leave standstill 5 minutes.Subsequently to the 80.0mL that adds water in iodine flask, make it mixing, then use normal sodium thiosulfate vs (0.1mol/L) titration, first being titrated to solution presents light yellow, then adds starch solution, as reaction indicator, be titrated to blue disappearance, what now reach is titration end-point.Consume number with the volume of hypo solution, calculate the peroxide value (POV) of grease.Computing formula:
POV＝(V1-V2)×0.001296M
-1×100 (3)
In formula: V1 is the normal sodium thiosulfate volume (mL) that sample consumes; V2 is the normal sodium thiosulfate volume (mL) that blank test consumes; M is sample quality (g).
Test in triplicate and calculate its mean value.
The preparation of sodium thiosulfate titrand: take sodium thiosulfate 26.0g, with natrium carbonicum calcinatum 0.20g, adds the cold-water solution newly boiled and becomes 1000mL, shake up, place 1 month, for subsequent use after filtering.
The demarcation of sodium thiosulfate titrand: accurately take the base weight potassium chromate 0.150g being dried to constant weight at 120 DEG C, put in iodine flask.The 50mL that adds water dissolves, add potassium iodide 2.0g, jolting is dissolved gently, adds dilute sulfuric acid 40mL, shakes up, in the dark place 10 minutes, the 250mL that adds water dilutes, and during terminal surely near with this drop, adds starch indicator solution 3mL, continue be titrated to blue disappearance and highlight green, and the result blank test of titration is corrected.The sodium thiosulfate vs (0.1mol/L) of every 1mL is equivalent to the potassium dichromate of 4.903mg.According to the consumption of this liquid consumption and potassium dichromate, calculate the actual concentrations of this liquid.Computing formula:
In formula: Ms is the quality (g) of potassium dichromate; V consumes by titration the volume (mL) of sodium thiosulfate vs; V
0consume by blank test the volume (mL) of sodium thiosulfate vs.
The detection method of the ganoderma lucidum spore oil oxidative rancidity based on Raman spectrum of the present invention, in step (1), described with 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the acid number of sample be horizontal ordinate mapping time, 1655cm
-1raman peaks integrated intensity and the acid number of its counter sample there is very good linear relationship, show to utilize Raman spectroscopy to carry out Quantitative detection (as shown in Figure 6) to the acid number produced in ganoderma lucidum spore oil oxidative rancidity process.
In step (1), described with 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the peroxide value of sample be horizontal ordinate mapping time, although 1655cm
-1the peroxide value of Raman peaks integrated intensity and its counter sample does not present linear relationship, but still can nonlinear fitting (software: Origin 8.0 be passed through, S matching, shown in Fig. 7 dotted line) or the mode (the method is existing ready-made mathematical method) of interpolate value Fast Measurement is carried out to the peroxide value of ganoderma lucidum spore oil.
Step (2), when detecting ganoderma lucidum spore oil test sample, because Raman spectrometer can Automatic continuous working sample, thus can realize the dynamic monitoring to sample.The key factor affecting ganoderma lucidum spore oil AV and POV is temperature, light, air, and the impact of temperature is greater than the impact of air and light.
According to the detection method of ganoderma lucidum spore oil oxidative rancidity that the present invention is based on Raman spectrum, can carry out the screening of Reishi sporule oil antioxidant, the method for described screening is:
Different several antioxidants is added in Reishi sporule oil samples one by one respectively, obtain the several Reishi sporule oil samples that with the addition of different antioxidant, some for gained samples are placed in one by one respectively 70 DEG C of uncovered preservations of thermostat lucifuge, stir every 24 ~ 36h and once mix, in 5 days, with the time gradient every 24h, often kind of sample is sampled, and detect with Raman spectrometer, the method of described detection is: get 20 ~ 200 μ L samples, be placed in kapillary or sample hose, put into Raman spectrometer sample cell, laser intensity is selected high-grade, laser irradiation time is set as 10s, automatically the calibration of environment parasitic light and baseline correction is carried out, sample determination is averaged for 5 times, obtain Raman spectrogram, and along with the passing of time gradient, often kind of sample all obtains a series of Raman spectrogram, 1655cm in calculated Raman spectrum figure
-1raman peaks integrated intensity, by the 1655cm calculated
-1raman peaks integrated intensity result contrasts with described acid number evaluation criterion figure, peroxide value evaluation criterion figure, often kind of sample obtains a series of acid number and peroxide value passed along with time gradient, according to the acid number obtained and peroxide value, the oxidative rancidity degree of ganoderma lucidum spore oil in different sample is evaluated, in identical time range, if the elevated-levels of acid number and peroxide value is less, illustrate that the oxidative rancidity degree of ganoderma lucidum spore oil is lower, then the effect of corresponding antioxidant is more excellent, thus draws the good and bad order of several different antioxidant.
Described antioxidant is selected from following several: TBHQ, VE, Tea Polyphenols; The interpolation quality of described antioxidant is 0.01% ~ 0.02% of ganoderma lucidum spore oil sample quality.
Compared with existing technology, beneficial effect of the present invention is as follows:
(1) in Raman spectrum, carbon-to-carbon double bond occurs with very strong characteristic peak usually, in finite concentration scope (in sample Reishi sporule oil content >=10ug/ml), the intensity at peak is directly proportional to the concentration of double bond, when double bond generation oxidative degradation is become sour, the intensity at peak declines, thus the palliating degradation degree of direct-detection carbon-to-carbon double bond can be carried out by the Characteristic Raman peak intensity measuring carbon-to-carbon double bond, direct quantitative analysis can be carried out like this, as shown in Figure 1 to the oxidative rancidity of ganoderma lucidum spore oil.
(2), in ganoderma lucidum spore oil Raman spectrogram, 1655cm is positioned at
-1the intensity (in sample Reishi sporule oil content>=10ug/ml) within the scope of finite concentration of double bond stretching vibration peak be directly proportional to the concentration of double bond, so can by detecting 1655cm
-1double bond peak intensity carry out the oxidative rancidity process of dynamic monitoring spore oil.Compared to the technological means (as nuclear-magnetism, high performance liquid chromatography, mass spectrum etc.) of other monitoring spore oil oxidative rancidity, Raman spectroscopy has more simply, directly, quick, the impact of oxidated intermediate product (as aldehyde, ketone) is little, sample without the need to advantages such as complicated pre-service, as shown in Figure 2.
(3) the time dependent curve that becomes sour of ganoderma lucidum spore oil can be obtained by the integrated intensity at double bond peak in Raman spectrogram to time mapping, by becoming sour, slope of a curve can obtain initial reaction rate constant, according to Arrhenius law, with reaction rate constant, the inverse of temperature is mapped, the apparent activation energy that can calculate oxidative rancidity reaction is Δ E=44.35kJ/mol, as shown in Figure 3, Figure 4.
(4) owing to adopting Raman spectroscopy simply, fast, directly can monitor ganoderma lucidum spore oil oxidative rancidity process, thus the rapid screening of Reishi sporule oil antioxidant can be carried out by high temperature Acceleration study.Further, according to the activation energy data obtained (Δ E=44.35kJ/mol), the shelf life of (20 DEG C) ganoderma lucidum spore oil can be calculated at room temperature, as shown in Figure 5.
(5) with the integrated intensity of ganoderma lucidum spore oil double bond Raman peaks with map known with the ganoderma lucidum spore oil acid number that standardized titration method records, no matter whether add antioxidant, integrated intensity and its acid number of double bond Raman peaks all have very good linear relationship, show to utilize Raman spectroscopy to carry out Quantitative detection to the acid number produced in spore oil oxidative rancidity process, as shown in Figure 6.With the integrated intensity of ganoderma lucidum spore oil double bond Raman peaks with map by the ganoderma lucidum spore oil peroxide value that standardized titration method records, although Raman peaks intensity and peroxide value do not present linear relationship, but still can nonlinear fitting (software: Origin8.0 be passed through, S matching, shown in Fig. 7 dotted line) or the mode (the method is existing ready-made mathematical method) of interpolate value Fast Measurement is carried out to the peroxide value of ganoderma lucidum spore oil.
Conventional acid-base titration method detects acid value of oil and fat and has following limitation: the terminal of (1) acid base titration depends on the faint change of indicator color, and between Different Individual, endpoint differs greatly, and special grease of working as is larger with color time error; (2) required oil sample consumption large (5 ~ 10g), solution preparation, demarcation, titration expend time in long (needing several hours); (3) chemical reagent needed for classic method and medicine many, need loaded down with trivial details preparation volumetric solution, be difficult to the requirement realizing field quick detection.And Raman spectroscopy is demarcated without the need to artificial terminal point determining and solution preparation, detection time fast (only needing a few minutes), few (the common sample pipe: 0.2mL with low cost of sample consumption, capillary sample hose: 0.02mL), simple and convenient, can field quick detection, thus make this detection method have sizable actual application prospect.
(4) accompanying drawing explanation
Fig. 1: the Raman spectrogram of ganoderma lucidum spore oil.1745.6cm
-1corresponding to the stretching vibration peak of carbonyl C=O in molecule, 1654.5cm
-1corresponding to the stretching vibration peak of unsaturated double-bond, 1439.2cm
-1corresponding to alkyl C-H bond CH scissoring vibration peak, 1300.9cm
-1corresponding to the deformation vibration peak of alkyl.In Raman spectrum, carbon-to-carbon double bond occurs with very strong characteristic peak usually, the intensity at peak is directly proportional to the concentration of double bond within the scope of finite concentration, when double bond generation oxidative degradation is become sour, the intensity at peak declines, thus the palliating degradation degree of direct-detection carbon-to-carbon double bond can be carried out by the Characteristic Raman peak intensity measuring carbon-to-carbon double bond, direct quantitative analysis can be carried out to the oxidative rancidity of ganoderma lucidum spore oil like this.
Fig. 2: in embodiment 2 under 50 DEG C of constant temperature, ganoderma lucidum spore oil exposes in atmosphere, and in 5 days, 7 days, 14 days, 21 days, 28 days, Raman spectrogram during sampling in 35 days as shown in Figure 2.
Fig. 3: the impact that in embodiment 2, temperature of reaction is reacted ganoderma lucidum spore oil oxidative rancidity.Obtain the time dependent curve that becomes sour of ganoderma lucidum spore oil with the integrated intensity at double bond peak in Raman spectrogram to time mapping, the curve that (10 DEG C, 35 DEG C, 50 DEG C, 70 DEG C) at differential responses temperature obtained becoming sour is plotted in Fig. 3.
Fig. 4: in embodiment 2, the lnk of ganoderma lucidum spore oil oxidative rancidity reaction maps to inverse temperature.Obtain initial reaction rate constant by the slope of a curve that becomes sour, according to Arrhenius law, with reaction rate constant, the inverse of temperature is mapped.
Fig. 5: the ganoderma lucidum spore oil oxidative rancidity change curve in time adding different antioxidant in embodiment 3.
Fig. 6: the integrated intensity relation of the acid number produced after ganoderma lucidum spore oil oxidative rancidity in embodiment 3 and double bond Raman peaks.No matter whether add antioxidant, integrated intensity and its acid number of double bond Raman peaks have very good linear relationship.
Fig. 7: the integrated intensity relation of the peroxide value produced after ganoderma lucidum spore oil oxidative rancidity in embodiment 3 and double bond Raman peaks.Although raman scattering intensity and peroxide value do not present linear relationship, but still can nonlinear fitting (software: Origin 8.0 be passed through, S matching, shown in Fig. 7 dotted line) or the mode (the method is existing ready-made mathematical method) of interpolate value Fast Measurement is carried out to the peroxide value of ganoderma lucidum spore oil.
(5) embodiment
With specific embodiment, the invention will be further described below, but protection scope of the present invention is not limited in this.
Embodiment 1: set up ganoderma lucidum spore oil acid number, peroxide value evaluation criterion figure
Get ganoderma lucidum spore oil, be placed in 70 DEG C of uncovered preservations of thermostat lucifuge, stir every 30h and once mix, in 24h, 48h, 72h, 96h, 120h samples respectively, after every sub-sampling, sample is detected, with standardized titration method (Chinese Pharmacopoeia Commission. Pharmacopoeia of People's Republic of China (). Beijing: China Medical Science Press, 2010. annex 54-55. and annex 56-57.) measure the acid number of Reishi sporule oil samples respectively, peroxide value, the Raman spectrogram of Reishi sporule oil samples is recorded with Raman spectrometer, obtain the acid number of series of samples, peroxide value, Raman spectrogram,
The detection method of the Raman spectrum of described ganoderma lucidum spore oil is: get 40 μ L Reishi sporule oil samples, be placed in kapillary or sample hose, put into Raman spectrometer (
advantage 785 type Near-infrared Raman spectroscopy instrument, DeltaNu company, the U.S., wavelength 785nm, laser power 120mW, resolution 4cm
-1, band NuScope digital microscope and XYZ three-dimensional objective table) and in sample cell, laser intensity is selected high-grade, laser irradiation time is set as 10s, automatically carry out the calibration of environment parasitic light and baseline correction, sample determination is averaged for 5 times times, obtains the Raman spectrogram of Reishi sporule oil samples;
With 1655cm in Raman spectrogram
-1raman peaks integrated intensity (Raman peaks integrated intensity calculates with the integrating function of the peak area in analysis software Grams, software calculates automatically, then copy or output data) for the acid number of ordinate, sample is horizontal ordinate mapping, obtain the acid number evaluation criterion figure of ganoderma lucidum spore oil; With 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the peroxide value of sample is horizontal ordinate mapping, obtains the peroxide value evaluation criterion figure of ganoderma lucidum spore oil;
Embodiment 2: the Raman spectrum of ganoderma lucidum spore oil acid number, peroxide value detects and the detection of dynamic of oxidative rancidity process fast
Under 50 DEG C of constant temperature, ganoderma lucidum spore oil exposes in atmosphere, samples respectively in 5 days, 7 days, 14 days, 21 days, 28 days, 35 days.After every sub-sampling, sample is detected, detection method: get 20 μ L Reishi sporule oil samples and be placed in 20 μ L kapillaries, put into Raman spectrometer (
advantage 785 type Near-infrared Raman spectroscopy instrument, DeltaNu company, the U.S., wavelength 785nm, laser power 120mW, resolution 4cm
-1, band NuScope digital microscope and XYZ three-dimensional objective table) and in sample cell, laser intensity is selected high-grade, and laser irradiation time is set as 10s, automatically carries out the calibration of environment parasitic light and baseline correction.Each sample determination is averaged for 5 times, obtains the Raman spectrogram of Reishi sporule oil samples, 1655cm in calculated Raman spectrum figure
-1raman peaks integrated intensity, by the 1655cm calculated
-1the acid number evaluation criterion figure that Raman peaks integrated intensity result obtains with embodiment 1 respectively, peroxide value evaluation criterion figure contrast, and obtain acid number and the peroxide value of sample, and then draw the oxidative rancidity degree evaluation result of Reishi sporule oil samples.
Raman spectrogram during sampling in 5 days, 7 days, 14 days, 21 days, 28 days, 35 days as shown in Figure 2.Can find out, when 50 DEG C, ganoderma lucidum spore oil just there occurs obvious oxidative rancidity from the 7th day, 14 days afterwards about 2/3 unsaturated double-bond acid destroy, illustrate that the speed of ganoderma lucidum spore oil oxidative rancidity is very fast at 50 DEG C of temperature.
With the integrated intensity at double bond peak in Raman spectrogram, the time dependent curve that becomes sour of ganoderma lucidum spore oil is obtained to time mapping, by at differential responses temperature (10 DEG C, 35 DEG C, 50 DEG C, 70 DEG C) curve that obtains becoming sour is plotted in Fig. 3, and can find out, the rate of temperature to spore oil oxidative rancidity is fairly obvious, when 10 DEG C, ganoderma lucidum spore oil is also little through 20 days oxidative rancidities, and when 70 DEG C through a few hours major part spore oil there occurs and become sour.Obtain initial reaction rate constant by the slope of a curve that becomes sour, according to Arrhenius law, map (Fig. 4) with reaction rate constant to the inverse of temperature, the apparent activation energy calculating oxidative rancidity reaction is Δ E=44.35kJ/mol.
Embodiment 3: utilize the detection method based on Raman spectrum to select the antioxidant of the most applicable ganoderma lucidum spore oil
Select TBHQ, VE, Tea Polyphenols 3 kinds of antioxidants, the dosage pressing 0.02wt% respectively adds.Accurately take 4 parts of ganoderma lucidum spore oils, portion does not add antioxidant as control sample, other three parts are added TBHQ, VE and Tea Polyphenols respectively, be placed in 70 DEG C of uncovered preservations of thermostat lucifuge, stir every 30h and once mix, regular sampling, measures the Raman spectrogram of ganoderma lucidum spore oil, 1655cm in calculated Raman spectrum figure with Raman spectrometer
-1raman peaks integrated intensity, by the 1655cm calculated
-1the acid number evaluation criterion figure that Raman peaks integrated intensity result obtains with embodiment 1 respectively, peroxide value evaluation criterion figure contrast, and obtain acid number and the peroxide value of sample, and then draw oxidative rancidity degree evaluation result
As shown in Figure 5, at 70 DEG C, monitoring is added 0.02wt% antioxidant and is not added the oxidative rancidity speed of antioxidant spore oil, obviously, oxidized very soon in the spore oil a few hours not adding antioxidant, antioxidant effect: vitamin E > Tea Polyphenols >TBHQ, add the spore oil of vitamin E after 6 days (double bond peak intensity declines 5%) just occur that slight oxidation is become sour.According to the activation energy data obtained above (Δ E=44.35kJ/mol), (20 DEG C) ganoderma lucidum spore oil shelf life can be calculated at room temperature and can reach about 90 days.In the environment of airtight low temperature, increase vitamin E consumption, can the shelf life of significant prolongation spore oil further.
Ganoderma lucidum spore oil shelf life computing method: known at 70 DEG C shelf life be 6 days (according to the curve that becomes sour, add the spore oil of vitamin E after 6 days, double bond peak intensity declines about 5%), according to Arrhenius formula, lnk=Δ E/RTln (k
70/ k
20)=Δ E/R* [1/ (70+273)-1/ (20+273)], calculates the ratio k of the reaction rate constant at two temperature
70/ k
20=15, so the shelf-life at 20 DEG C is within 6 days, be multiplied by 15 to equal 90 days.
With the integrated intensity of ganoderma lucidum spore oil double bond Raman peaks with map with the ganoderma lucidum spore oil acid number that standardized titration method is measured, as shown in Figure 6, can find out, no matter whether add antioxidant, integrated intensity and its acid number of double bond Raman peaks have very good linear relationship, show to utilize Raman spectroscopy to carry out Quantitative detection to the acid number produced in ganoderma lucidum spore oil oxidative rancidity process.Compared to conventional acid-base titration method, Raman spectroscopy is simple, convenient, fast, few by sample amount, with low cost, thus makes the method have sizable actual application prospect.
Use the same method, with the integrated intensity of ganoderma lucidum spore oil double bond Raman peaks with map by the ganoderma lucidum spore oil peroxide value that standardized titration method is measured, as shown in Figure 7.Although raman scattering intensity and peroxide value do not present linear relationship, but still can nonlinear fitting (software: Origin 8.0 be passed through, S matching, shown in Fig. 7 dotted line) or the mode (the method is existing ready-made mathematical method) of interpolate value Fast Measurement is carried out to the peroxide value of ganoderma lucidum spore oil.
Claims (1)
1., based on a detection method for the ganoderma lucidum spore oil oxidative rancidity of Raman spectrum, the oxidative rancidity degree of described ganoderma lucidum spore oil, using the acid number of ganoderma lucidum spore oil, peroxide value as evaluation index, is characterized in that, described detection method comprises the steps:
(1) ganoderma lucidum spore oil acid number, peroxide value evaluation criterion figure is set up
Get ganoderma lucidum spore oil, be placed in 70 DEG C of uncovered preservations of thermostat lucifuge, stir every 24 ~ 36h and once mix, in 5 days, sample with the time gradient every 24 hours, after every sub-sampling, sample is detected, measure acid number, the peroxide value of Reishi sporule oil samples by standardized titration method respectively, record the Raman spectrogram of Reishi sporule oil samples with Raman spectrometer, obtain acid number, peroxide value, the Raman spectrogram of series of samples;
The detection method of the Raman spectrum of described ganoderma lucidum spore oil is: get 20 ~ 200 μ L Reishi sporule oil samples, be placed in kapillary or sample hose, put into Raman spectrometer sample cell, laser intensity is selected high-grade, laser irradiation time is set as 10s, automatically carries out the calibration of environment parasitic light and baseline correction, and sample determination is averaged for 5 times times, obtain the Raman spectrogram of Reishi sporule oil samples, 1655cm in calculated Raman spectrum figure
-1raman peaks integrated intensity;
With 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the acid number of sample is horizontal ordinate mapping, obtains the acid number evaluation criterion figure of ganoderma lucidum spore oil; With 1655cm in Raman spectrogram
-1raman peaks integrated intensity be ordinate, the peroxide value of sample is horizontal ordinate mapping, obtains the peroxide value evaluation criterion figure of ganoderma lucidum spore oil;
(2) detection of test sample
Get 20 ~ 200 μ L ganoderma lucidum spore oil test samples, be placed in kapillary or sample hose, put into Raman spectrometer sample cell, laser intensity is selected high-grade, laser irradiation time is set as 10s, automatically carry out the calibration of environment parasitic light and baseline correction, sample determination is averaged for 5 times, obtains the Raman spectrogram of ganoderma lucidum spore oil test sample; 1655cm in calculated Raman spectrum figure
-1raman peaks integrated intensity, by the 1655cm calculated
-1acid number evaluation criterion figure, peroxide value evaluation criterion figure that Raman peaks integrated intensity result obtains with step (1) respectively contrast, obtain acid number and the peroxide value of test sample, and then draw the oxidative rancidity degree evaluation result of ganoderma lucidum spore oil test sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510372342.0A CN104931482A (en) | 2015-06-26 | 2015-06-26 | Detection method for oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510372342.0A CN104931482A (en) | 2015-06-26 | 2015-06-26 | Detection method for oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104931482A true CN104931482A (en) | 2015-09-23 |
Family
ID=54118754
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510372342.0A Pending CN104931482A (en) | 2015-06-26 | 2015-06-26 | Detection method for oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104931482A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105628681A (en) * | 2016-04-11 | 2016-06-01 | 惠州市食品药品检验所 | Identification method of ganoderma lucidum spore oil |
| CN106006764A (en) * | 2016-05-12 | 2016-10-12 | 徐靖才 | Method for preparing ordered mesopore nickel oxide gas-sensing nano material |
| CN106153601A (en) * | 2016-10-08 | 2016-11-23 | 江南大学 | A kind of method based on SERS detection grease oxide in trace quantities since |
| CN106323942A (en) * | 2016-09-08 | 2017-01-11 | 福建师范大学 | Fast detecting method of grease peroxidation value |
| CN108196015A (en) * | 2018-02-06 | 2018-06-22 | 吉林农业大学 | A kind of food with filling automated detection method |
| CN109142654A (en) * | 2018-08-07 | 2019-01-04 | 广东百美倚德生物科技有限公司 | A method of determining the rancid degree of soyabean lecithin oil |
| CN109324032A (en) * | 2018-11-30 | 2019-02-12 | 厦门谱识科仪有限公司 | A kind of surface-enhanced Raman spectroscopy for realizing food safety rapid screening |
| CN109856230A (en) * | 2019-01-30 | 2019-06-07 | 山东博戎伝创信息科技有限公司 | Organic compound residue analysis method and device and intelligent monitoring system thereof |
| CN110736730A (en) * | 2019-10-31 | 2020-01-31 | 楚雄师范学院 | screening process of obtaining industrial hemp plant with high cannabidiol content |
| CN111562250A (en) * | 2020-05-26 | 2020-08-21 | 河北省食品检验研究院 | Method for rapidly detecting ganoderic acid G in ganoderma lucidum spore oil |
| CN111562251A (en) * | 2020-05-26 | 2020-08-21 | 河北省食品检验研究院 | Method for rapidly detecting ganoderic acid B in ganoderma lucidum spore powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2358321A1 (en) * | 2000-09-29 | 2002-03-29 | Kraft Foods Holdings, Inc. | Method and composition which inhibits the oxidation of omega-3- and omega-6 polyunsaturated lipids |
| CN1931195A (en) * | 2005-09-12 | 2007-03-21 | 吴逸芳 | Glossy ganoderma spore oil and its supercritical prepn process |
| CN103398970A (en) * | 2013-07-24 | 2013-11-20 | 骆驰 | Method for qualitatively and quantitatively analyzing edible oil and further detecting hogwash oil |
| CN103645171A (en) * | 2013-12-03 | 2014-03-19 | 深圳市疾病预防控制中心 | Method for detecting gutter oil based on Raman spectrometry |
-
2015
- 2015-06-26 CN CN201510372342.0A patent/CN104931482A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2358321A1 (en) * | 2000-09-29 | 2002-03-29 | Kraft Foods Holdings, Inc. | Method and composition which inhibits the oxidation of omega-3- and omega-6 polyunsaturated lipids |
| CN1931195A (en) * | 2005-09-12 | 2007-03-21 | 吴逸芳 | Glossy ganoderma spore oil and its supercritical prepn process |
| CN103398970A (en) * | 2013-07-24 | 2013-11-20 | 骆驰 | Method for qualitatively and quantitatively analyzing edible oil and further detecting hogwash oil |
| CN103645171A (en) * | 2013-12-03 | 2014-03-19 | 深圳市疾病预防控制中心 | Method for detecting gutter oil based on Raman spectrometry |
Non-Patent Citations (3)
| Title |
|---|
| 王青青 等: "灵芝孢子油的氧化稳定性", 《福建中医药大学学报》 * |
| 能静 等: "基于拉曼光谱法的灵芝孢子油氧化酸败检测新技术", 《食品科学》 * |
| 高宇杰 等: "超临界CO2萃取灵芝孢子油及其挥发性成分分析", 《食品科学》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105628681A (en) * | 2016-04-11 | 2016-06-01 | 惠州市食品药品检验所 | Identification method of ganoderma lucidum spore oil |
| CN106006764A (en) * | 2016-05-12 | 2016-10-12 | 徐靖才 | Method for preparing ordered mesopore nickel oxide gas-sensing nano material |
| CN106006764B (en) * | 2016-05-12 | 2017-09-15 | 中国计量大学 | A kind of preparation method of order mesoporous nickel oxide gas sensitization nano material |
| CN106323942A (en) * | 2016-09-08 | 2017-01-11 | 福建师范大学 | Fast detecting method of grease peroxidation value |
| CN106153601B (en) * | 2016-10-08 | 2019-01-22 | 江南大学 | A method of grease oxide in trace quantities since is detected based on Surface enhanced Raman spectroscopy |
| CN106153601A (en) * | 2016-10-08 | 2016-11-23 | 江南大学 | A kind of method based on SERS detection grease oxide in trace quantities since |
| CN108196015A (en) * | 2018-02-06 | 2018-06-22 | 吉林农业大学 | A kind of food with filling automated detection method |
| CN109142654A (en) * | 2018-08-07 | 2019-01-04 | 广东百美倚德生物科技有限公司 | A method of determining the rancid degree of soyabean lecithin oil |
| CN109324032A (en) * | 2018-11-30 | 2019-02-12 | 厦门谱识科仪有限公司 | A kind of surface-enhanced Raman spectroscopy for realizing food safety rapid screening |
| CN109856230A (en) * | 2019-01-30 | 2019-06-07 | 山东博戎伝创信息科技有限公司 | Organic compound residue analysis method and device and intelligent monitoring system thereof |
| CN109856230B (en) * | 2019-01-30 | 2021-09-21 | 山东博戎伝创信息科技有限公司 | Organic compound residue analysis method and device and intelligent monitoring system thereof |
| CN110736730A (en) * | 2019-10-31 | 2020-01-31 | 楚雄师范学院 | screening process of obtaining industrial hemp plant with high cannabidiol content |
| CN111562250A (en) * | 2020-05-26 | 2020-08-21 | 河北省食品检验研究院 | Method for rapidly detecting ganoderic acid G in ganoderma lucidum spore oil |
| CN111562251A (en) * | 2020-05-26 | 2020-08-21 | 河北省食品检验研究院 | Method for rapidly detecting ganoderic acid B in ganoderma lucidum spore powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104931482A (en) | Detection method for oxidation rancidity of ganoderma lucidum spore oil based on Raman spectrum | |
| CN103245628B (en) | The method for quick of food plant oil quality | |
| Pénicaud et al. | Oxygen quantification methods and application to the determination of oxygen diffusion and solubility coefficients in food | |
| CN102435749A (en) | Liquid stable kit for measuring beta-hydroxybutyric acid by cyclic enzyme method | |
| CN103207152A (en) | Method for detecting sulfur dioxide in plant-derived food | |
| CN106153601A (en) | A kind of method based on SERS detection grease oxide in trace quantities since | |
| CN103134767A (en) | Method for liquor quality identification through infrared spectrum revision | |
| CN103344588A (en) | Method for detecting trace concentration of copper ions | |
| CN104764699A (en) | Method for determination of edible oil acid value | |
| CN104390918A (en) | Noninvasive detection system and method of diabetes and complications of diabetes | |
| CN110031558A (en) | The rapid detection method of Fatty Acids from Vegetable Oil and squalene | |
| WO2019165734A1 (en) | Rapid combined detection device for detecting deterioration degree of frying oil and detection method therefor | |
| Arroyo et al. | Capillary microfluidic platform for sulfite determination in wines | |
| Li et al. | A benzothiazole-salt-based fluorescent probe for precise monitoring the changes of pH and viscosity | |
| CN204128960U (en) | A kind of drinks quality sense organ classification quick analytic instrument | |
| CN106383106A (en) | Quick detection method of trace antioxidant in grease | |
| CN103196851A (en) | Measuring method of arsenic content of glyceryl triacetate | |
| CN201788153U (en) | Pesticide residue detector integrated with micro electronic balance | |
| CN103267733A (en) | Novel method for detecting scented tea antioxidant activity | |
| Kruatian et al. | Simple spectrophotometric method for determination of iodine value of vegetable oils | |
| IT201800003475A1 (en) | Procedure for determining the antioxidant capacity of a biological sample and relative kit. | |
| CN102854228B (en) | Edible oil peroxidation value determination method based on conductivity | |
| CN102608050B (en) | Identification and quantitative analysis method for refined gutter oil | |
| CN110749673A (en) | Primary olive oil comparison fingerprint spectrum and construction method and application thereof | |
| CN103091305A (en) | Method for detecting quinolone antibiotic by means of electrochemical luminescence |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150923 |
|
| WD01 | Invention patent application deemed withdrawn after publication |