CN102297908A - Method for detecting illegal cooking oil - Google Patents
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- CN102297908A CN102297908A CN2011101314924A CN201110131492A CN102297908A CN 102297908 A CN102297908 A CN 102297908A CN 2011101314924 A CN2011101314924 A CN 2011101314924A CN 201110131492 A CN201110131492 A CN 201110131492A CN 102297908 A CN102297908 A CN 102297908A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000008162 cooking oil Substances 0.000 title abstract 5
- 239000003921 oil Substances 0.000 claims abstract description 89
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims abstract description 58
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 28
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 27
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 24
- 229930195729 fatty acid Natural products 0.000 claims abstract description 24
- 239000000194 fatty acid Substances 0.000 claims abstract description 24
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 14
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims abstract description 14
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 10
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims description 55
- 239000007789 gas Substances 0.000 claims description 39
- 238000001819 mass spectrum Methods 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 13
- 229940005605 valeric acid Drugs 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 9
- 238000004949 mass spectrometry Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract 3
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 abstract 1
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 66
- 238000004332 deodorization Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000008157 edible vegetable oil Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 238000011088 calibration curve Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 241000251468 Actinopterygii Species 0.000 description 2
- 241001372210 Gobioides broussonnetii Species 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 235000021190 leftovers Nutrition 0.000 description 2
- 239000004006 olive oil Substances 0.000 description 2
- 235000008390 olive oil Nutrition 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 235000021391 short chain fatty acids Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- RUVINXPYWBROJD-ONEGZZNKSA-N trans-anethole Chemical compound COC1=CC=C(\C=C\C)C=C1 RUVINXPYWBROJD-ONEGZZNKSA-N 0.000 description 2
- 235000002566 Capsicum Nutrition 0.000 description 1
- 240000008574 Capsicum frutescens Species 0.000 description 1
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 description 1
- VMYXUZSZMNBRCN-AWEZNQCLSA-N Curcumene Natural products CC(C)=CCC[C@H](C)C1=CC=C(C)C=C1 VMYXUZSZMNBRCN-AWEZNQCLSA-N 0.000 description 1
- ZFMSMUAANRJZFM-UHFFFAOYSA-N Estragole Chemical compound COC1=CC=C(CC=C)C=C1 ZFMSMUAANRJZFM-UHFFFAOYSA-N 0.000 description 1
- 239000005770 Eugenol Substances 0.000 description 1
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 description 1
- 229940011037 anethole Drugs 0.000 description 1
- 239000001390 capsicum minimum Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- -1 dihydro isoesdragol Chemical compound 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960002217 eugenol Drugs 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- RUVINXPYWBROJD-UHFFFAOYSA-N para-methoxyphenyl Natural products COC1=CC=C(C=CC)C=C1 RUVINXPYWBROJD-UHFFFAOYSA-N 0.000 description 1
- 235000015277 pork Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- VMYXUZSZMNBRCN-UHFFFAOYSA-N α-curcumene Chemical compound CC(C)=CCCC(C)C1=CC=C(C)C=C1 VMYXUZSZMNBRCN-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for detecting illegal cooking oil. The method comprises steps that: 1, an oil sample requiring detection is added into a headspace bottle, the headspace bottle is shaken under a temperature of 40 to 150 DEG C, and is then balanced for 10min to 120min; 2, upper-layer gas in the headspace bottle is taken by using an injector after balancing, the taken gas sample is delivered into a gas chromatograph-mass spectrometer, and a gas chromatography-mass spectrometry spectrogram is obtained under configured chromatographic and mass spectrometric conditions; 3, qualitative analysis is carried out upon the gas chromatography-mass spectrometry spectrogram with an NIST mass spectrogram library; when fatty acids are detected in the oil sample requiring detection, it is determined that the oil sample is illegal cooking oil, or that the oil sample contains illegal cooking oil, wherein the fatty acids are one, two or more selected from acetic acid, propionic acid, butanoic acid, butylcarboxylic acid, and hexanoic acid. The method provided by the invention has good accuracy, and is suitable for detecting all types of illegal cooking oil.
Description
Technical field
The present invention relates to a kind of method that detects waste oil.
Background technology
Waste oil mainly comprises three major types: the waste oil of (1) narrow sense, be about in the sewer greasy floating thing or with leftovers, the oil of leftovers of hotel, restaurant through simply processing, extracting.(2) oil that extracts by pork inferior, haslet, pigskin processing.(3) after the oily access times that are used for fried food surpass certain number of times, be repeated again to use or toward wherein adding the oil of reusing behind some fresh oils.Health ministry, the State Administration for Industry and Commerce, Environmental Protection Administration and the Ministry of Construction in 2002 unite in the issue " regulation of the discarded edible oil and fat management of food production or marketing unit " and spell out: be re-used as edible oil and fat after must not waste grease processing and use or sell.
The method of at present the most general detection waste oil is an electrical conductivity method, but surrounding environment that conductivity indices is contacted with sample when measuring and the water that is extracted have bigger correlativity, therefore the accuracy of this method is also bad, can only be as a preliminary discrimination method, the prompting sample may contain waste oil.
Chinese patent literature CN101852783A discloses the method that a kind of headspace solid-phase microextraction-gas chromatography combined with mass spectrometry detects hogwash fat, thereby this method is by detecting in the oil sample whether contain chavicol methyl ether, dihydro isoesdragol, anethole, eugenol or/and the curcumene spice judges whether this oil sample is hogwash fat or contains hogwash fat.Because on Sichuan, Chongqing and other places, the locals likes eating peppery, makes spices such as all can containing capsicum in the daily swill, makes like this can contain mentioned component in the hogwash fat.But much local for China, not necessarily can contain these compositions in the hogwash fat, so this method can't detect the hogwash fat that does not contain these compositions.
Summary of the invention
The objective of the invention is to address the above problem, provide that a kind of accuracy is good, the method for the detection waste oil that is applicable to all waste oils.
Technical conceive of the present invention is: the waste oil wide material sources, and complicated component, even through repeatedly processing, a lot of micro-volatile ingredients can not effectively be removed.The present invention is by detecting the micro-volatile constituent in the waste oil, and select for use nearly hundred kinds of normal edible vegetable oils to contrast, found out difference component---the fatty acid such as butyric acid of waste oil with normal edible vegetable oil, wherein butyric acid is the most important characteristic index, detects and can judge also under the NF situation of other fatty acid that oil sample to be measured is a waste oil at butyric acid.Also can infer the ratio of blending of blending waste oil simultaneously, the minimum waste oil of blending that can detect 1% addition according to butyric acid content.
The technical scheme that realizes the object of the invention is: a kind of method that detects waste oil, in detecting oil sample to be measured, contain fatty acid, and judge that then this oil sample to be measured is waste oil or contains waste oil; Described fatty acid is a kind of or two kinds or more of in acetate, propionic acid, butyric acid, valeric acid, the caproic acid.
Static headspace analysis-the GC-MS(gas chromatography-mass spectrography) of described detection method.
Described fatty acid is butyric acid.
The method of above-mentioned detection waste oil has following steps: 1. oil sample to be measured is joined in the head space bottle, shake the head space bottle under 40 ℃～150 ℃ temperature, then balance 10min～120min; 2. use syringe draw step 1. the gas sampling on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), under chromatographic condition of setting and mass spectrum condition, obtain the gas chromatography-mass spectrography spectrogram; 3. by NIST mass spectrum picture library the gas chromatography-mass spectrography spectrogram that 2. step obtains is carried out qualitative analysis; In detecting oil sample to be measured, contain fatty acid, judge that then this oil sample to be measured is waste oil or contains waste oil; Described fatty acid is a kind of or two kinds or more of in acetate, propionic acid, butyric acid, valeric acid, the caproic acid.
Described fatty acid is butyric acid.
The volume of the head space bottle of above-mentioned steps described in 1. is 10mL or 20mL, and described oil sample to be measured is 1mL～10mL; The step 2. gas of middle sample introduction is 20 μ L～500 μ L.
The 2. middle chromatographic condition of setting of above-mentioned steps is: 230 ℃ of injector temperatures; Chromatographic column: HP-5ms(0.25mm * 30m * 0.25 μ m); Carrier gas is a helium, and flow velocity is 1.0mL/min; Column temperature adopts temperature programme.
The temperature-programmed mode of being told is: 40 ℃ of initial temperatures keep 4min; Rise to 80 ℃ with 5 ℃/min speed, keep 2min; Rise to 220 ℃ with 20 ℃/min speed.
The 2. middle mass spectrum condition of setting of above-mentioned steps is: 280 ℃ of chromatography-mass spectroscopy interface temperature; 150 ℃ of ion source temperatures; 230 ℃ of level Four bar temperature; The ionization mode is EI; The mass scanning scope is 33amu～450amu; Scan mode is the full scan pattern; Ionizing energy is 70 eV; Electron-multiplier voltage is 1.1kV; Solvent delay is 0min.
The good effect that the present invention has: (1) method of the present invention not only can detect waste oil, and can detect the waste oil of decoloration and deodorization, can also detect and blend waste oil, the minimum waste oil of blending that can detect 1% addition.(2) method speed of the present invention is fast, can finish the detection of a sample about 20min, and the automaticity height is less demanding to operating personnel.(3) method amount of samples of the present invention is few, need not solvent, Environmental Safety.(4) method good reproducibility of the present invention, resolution is good, and accuracy is good, and minimal detectable concentration reaches 10 μ g/kg, and the range of linearity can reach 4 orders of magnitude.
Description of drawings
GC-MS total ion current figure in the gas chromatography-mass spectrography spectrogram that Fig. 1 obtains for embodiment 1;
GC-MS total ion current figure in the gas chromatography-mass spectrography spectrogram that Fig. 2 obtains for embodiment 2;
GC-MS total ion current figure in the gas chromatography-mass spectrography spectrogram that Fig. 3 obtains for Comparative Examples 1.
Embodiment
(embodiment 1)
The oil sample to be measured of present embodiment is a waste oil.
The detection method of present embodiment has following steps:
1. the waste oil with 10mL joins in the head space bottle of 20mL, covers bottle cap, is heated to 100 ℃ and also shakes the head space bottle strongly, and balance 50min is stand-by after stablizing then;
2. use syringe draw step 1. the gas 80 μ L sample introductions on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), obtain the gas chromatography-mass spectrography spectrogram under chromatographic condition of setting and mass spectrum condition, GC-MS total ion current figure wherein sees Fig. 1.
The chromatographic condition that sets is: 230 ℃ of injector temperatures; Chromatographic column: HP-5ms(0.25mm * 30m * 0.25 μ m); Carrier gas is helium (purity 99.99%), and flow velocity is 1.0mL/min; Column temperature adopts temperature programme: 40 ℃ of initial temperatures keep 4min; Rise to 80 ℃ with 5 ℃/min speed, keep 2min; Rise to 220 ℃ with 20 ℃/min speed.
The mass spectrum condition that sets is: 280 ℃ of chromatography-mass spectroscopy interface temperature; 150 ℃ of ion source temperatures; 230 ℃ of level Four bar temperature; The ionization mode is EI; The mass scanning scope is 33amu～450amu; Scan mode is the full scan pattern; Ionizing energy is 70 eV; Electron-multiplier voltage is 1.1kV; Solvent delay is 0min.
3. by NIST mass spectrum picture library 2. step is obtained the gas chromatography-mass spectrography spectrogram and carry out qualitative analysis.The result shows (seeing Table 1): contain fatty acid such as acetate, propionic acid, butyric acid, valeric acid, caproic acid in this waste oil, the content that adopts calibration curve method to calculate acetate is 2.5mg/kg, the content of propionic acid is 7.6mg/kg, the content of butyric acid is 24.0mg/kg, the content of valeric acid is 5.9mg/kg, and the content of caproic acid is 1.1mg/kg.
(embodiment 2)
The oil sample to be measured of present embodiment is the waste oil of decoloration and deodorization.
The detection method of present embodiment has following steps:
1. the waste oil with the decoloration and deodorization of 10mL joins in the head space bottle of 20mL, covers bottle cap, is heated to 80 ℃ and shake the head space bottle strongly, balance 40min then, and stable back is stand-by;
2. use syringe draw step 1. the gas 70 μ L sample introductions on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), obtain the gas chromatography-mass spectrography spectrogram under chromatographic condition of setting and mass spectrum condition, GC-MS total ion current figure wherein sees Fig. 2.
The chromatographic condition that sets of present embodiment is identical with embodiment 1 with the mass spectrum condition.
3. by NIST mass spectrum picture library 2. step is obtained the gas chromatography-mass spectrography spectrogram and carry out qualitative analysis.The result shows (seeing Table 1): contain butyric acid in the waste oil of this decoloration and deodorization but do not contain fatty acid such as acetate, propionic acid, valeric acid, caproic acid, the content that adopts calibration curve method to calculate butyric acid is 7.1mg/kg.
(embodiment 3)
Present embodiment is that oil sample to be measured is an edible oil of blending the waste oil of decoloration and deodorization, and wherein the content of the waste oil of decoloration and deodorization is the 1%(percent by volume, down together).
The detection method of present embodiment has following steps:
1. the oil sample to be measured with 10mL joins in the head space bottle of 20mL, covers bottle cap, is heated to 60 ℃ and also shakes the head space bottle strongly, and balance 30min is stand-by after stablizing then;
2. use syringe draw step 1. the gas 60 μ L sample introductions on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), under chromatographic condition of setting and mass spectrum condition, obtain the gas chromatography-mass spectrography spectrogram.
The chromatographic condition that sets of present embodiment is identical with embodiment 1 with the mass spectrum condition.
3. by NIST mass spectrum picture library 2. step is obtained the gas chromatography-mass spectrography spectrogram and carry out qualitative analysis.The result shows (seeing Table 1): contain butyric acid in this oil sample to be measured but do not contain fatty acid such as acetate, propionic acid, valeric acid, caproic acid, the content that adopts calibration curve method to calculate butyric acid is 0.2mg/kg.
(embodiment 4)
Present embodiment is substantially the same manner as Example 3, and difference is: oil sample to be measured is an edible oil of blending the waste oil of decoloration and deodorization, and wherein the content of the waste oil of decoloration and deodorization is 5%.The result shows: contain butyric acid in this oil sample to be measured but do not contain fatty acid such as acetate, propionic acid, valeric acid, caproic acid, the content of butyric acid is 0.8mg/kg.
(embodiment 5)
Present embodiment is substantially the same manner as Example 3, and difference is: oil sample to be measured is an edible oil of blending the waste oil of decoloration and deodorization, and wherein the content of the waste oil of decoloration and deodorization is 10%.The result shows: contain butyric acid in this oil sample to be measured but do not contain fatty acid such as acetate, propionic acid, valeric acid, caproic acid, the content of butyric acid is 1.3mg/kg.
(Comparative Examples 1)
The detection method of this Comparative Examples has following steps:
1. the golden imperial fish soybean oil with 10mL joins in the head space bottle of 20mL, covers bottle cap, is heated to 80 ℃ and also shakes the head space bottle strongly, and balance 40min is stand-by after stablizing then;
2. use syringe draw step 1. the gas 80 μ L sample introductions on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), obtain the gas chromatography-mass spectrography spectrogram under chromatographic condition of setting and mass spectrum condition, GC-MS total ion current figure wherein sees Fig. 3.
The chromatographic condition that sets of this Comparative Examples is identical with embodiment 1 with the mass spectrum condition.
3. by NIST mass spectrum picture library 2. step is obtained the gas chromatography-mass spectrography spectrogram and carry out qualitative analysis.The result shows (seeing Table 1): do not contain fatty acid such as acetate, propionic acid, butyric acid, valeric acid, caproic acid in this gold dragon fish soybean oil.
(Comparative Examples 2)
The detection method of this Comparative Examples has following steps:
1. the golden imperial fish blending stock with 4mL joins in the head space bottle of 10mL, covers bottle cap, is heated to 60 ℃ and also shakes the head space bottle strongly, and balance 30min is stand-by after stablizing then;
2. use syringe draw step 1. the gas 40 μ L sample introductions on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), under chromatographic condition of setting and mass spectrum condition, obtain the gas chromatography-mass spectrography spectrogram.
The chromatographic condition that sets of this Comparative Examples is identical with embodiment 1 with the mass spectrum condition.
3. by NIST mass spectrum picture library 2. step is obtained the gas chromatography-mass spectrography spectrogram and carry out qualitative analysis.The result shows (seeing Table 1): do not contain fatty acid such as acetate, propionic acid, butyric acid, valeric acid, caproic acid in this gold dragon fish blending stock.
(Comparative Examples 3)
The detection method of this Comparative Examples has following steps:
1. the olive oil with 8mL joins in the head space bottle of 20mL, covers bottle cap, is heated to 100 ℃ and also shakes the head space bottle strongly, and balance 50min is stand-by after stablizing then;
2. use syringe draw step 1. the gas 150 μ L sample introductions on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), under chromatographic condition of setting and mass spectrum condition, obtain the gas chromatography-mass spectrography spectrogram.
The chromatographic condition that sets of this Comparative Examples is identical with embodiment 1 with the mass spectrum condition.
3. by NIST mass spectrum picture library 2. step is obtained the gas chromatography-mass spectrography spectrogram and carry out qualitative analysis.The result shows (seeing Table 1): do not contain fatty acid such as acetate, propionic acid, butyric acid, valeric acid, caproic acid in this olive oil.
As can be seen from Table 1, all do not contain above-mentioned five kinds of SCFAs in the daily edible oil, then all contain these SCFAs in the waste oil, but in the waste oil of decoloration and deodorization, except butyric acid, other SCFA has all been removed by process for refining, so butyric acid is the evident difference of waste oil and daily edible oil.As long as in oil sample, detect butyric acid, can assert that then this oil sample contains waste oil, and if can also detect other SCFA, can assert that then this oil sample is without refining waste oil.
Claims (9)
1. a method that detects waste oil is characterized in that: contain fatty acid in detecting oil sample to be measured, judge that then this oil sample to be measured is waste oil or contains waste oil; Described fatty acid is a kind of or two kinds or more of in acetate, propionic acid, butyric acid, valeric acid, the caproic acid.
2. the method for detection waste oil according to claim 1 is characterized in that: described detection method is static headspace analysis-GC-MS(gas chromatography-mass spectrography).
3. the method for detection waste oil according to claim 1 and 2 is characterized in that: described fatty acid is butyric acid.
4. the method for detection waste oil according to claim 2 is characterized in that having following steps:
1. oil sample to be measured is joined in the head space bottle, under 40 ℃～150 ℃ temperature, shake the head space bottle, then balance 10min～120min;
2. use syringe draw step 1. the gas sampling on the head space bottle upper strata after the balance to gas chromatograph-mass spectrometer (GCMS), under chromatographic condition of setting and mass spectrum condition, obtain the gas chromatography-mass spectrography spectrogram;
3. by NIST mass spectrum picture library the gas chromatography-mass spectrography spectrogram that 2. step obtains is carried out qualitative analysis; In detecting oil sample to be measured, contain fatty acid, judge that then this oil sample to be measured is waste oil or contains waste oil; Described fatty acid is a kind of or two kinds or more of in acetate, propionic acid, butyric acid, valeric acid, the caproic acid.
5. the method for detection waste oil according to claim 4 is characterized in that: described fatty acid is butyric acid.
6. according to the method for claim 4 or 5 described detection waste oils, it is characterized in that: the volume of the head space bottle of step described in 1. is 10mL or 20mL, and described oil sample to be measured is 1mL～10mL; The step 2. gas of middle sample introduction is 20 μ L～500 μ L.
7. according to the method for claim 4 or 5 described detection waste oils, it is characterized in that: the 2. middle chromatographic condition of setting of step is: 230 ℃ of injector temperatures; Chromatographic column: HP-5ms(0.25mm * 30m * 0.25 μ m); Carrier gas is a helium, and flow velocity is 1.0mL/min; Column temperature adopts temperature programme.
8. the method for detection waste oil according to claim 7 is characterized in that: the temperature-programmed mode of being told is: 40 ℃ of initial temperatures keep 4min; Rise to 80 ℃ with 5 ℃/min speed, keep 2min; Rise to 220 ℃ with 20 ℃/min speed.
9. according to the method for claim 4 or 5 described detection waste oils, it is characterized in that: the 2. middle mass spectrum condition of setting of step is: 280 ℃ of chromatography-mass spectroscopy interface temperature; 150 ℃ of ion source temperatures; 230 ℃ of level Four bar temperature; The ionization mode is EI; The mass scanning scope is 33amu～450amu; Scan mode is the full scan pattern; Ionizing energy is 70 eV; Electron-multiplier voltage is 1.1kV; Solvent delay is 0min.
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| CN102636554A (en) * | 2012-04-24 | 2012-08-15 | 河北工业大学 | Method for identifying drainage oil |
| CN102721794A (en) * | 2012-06-26 | 2012-10-10 | 郑州炜盛电子科技有限公司 | Fast detection method of illegal cooking oil |
| CN102841171A (en) * | 2012-09-03 | 2012-12-26 | 湖南农业大学 | Detection method for tea seed oil adulteration based on ratio of main fatty acids |
| CN103134921A (en) * | 2012-12-27 | 2013-06-05 | 北京智云达科技有限公司 | Illegal cooking oil colloidal gold fast measuring card |
| CN103512990A (en) * | 2012-06-30 | 2014-01-15 | 中国科学院大连化学物理研究所 | Method for identifying plant-derived waste oil by adopting trace fatty acid |
| CN103798414A (en) * | 2012-11-13 | 2014-05-21 | 杨晓林 | Edible oil containing molecular markers as well as preparation method and application thereof |
| CN104198639A (en) * | 2014-09-09 | 2014-12-10 | 中国石油化工股份有限公司 | Quantitative analysis method for micromolecular organic acids in fluid extracted from oil field |
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| CN102636554A (en) * | 2012-04-24 | 2012-08-15 | 河北工业大学 | Method for identifying drainage oil |
| CN102721794A (en) * | 2012-06-26 | 2012-10-10 | 郑州炜盛电子科技有限公司 | Fast detection method of illegal cooking oil |
| CN102721794B (en) * | 2012-06-26 | 2015-07-01 | 郑州炜盛电子科技有限公司 | Fast detection method of illegal cooking oil |
| CN103512990A (en) * | 2012-06-30 | 2014-01-15 | 中国科学院大连化学物理研究所 | Method for identifying plant-derived waste oil by adopting trace fatty acid |
| CN103512990B (en) * | 2012-06-30 | 2015-11-18 | 中国科学院大连化学物理研究所 | Adopt the method for trace fatty acid differential plant source property waste oil |
| CN102841171A (en) * | 2012-09-03 | 2012-12-26 | 湖南农业大学 | Detection method for tea seed oil adulteration based on ratio of main fatty acids |
| CN103798414B (en) * | 2012-11-13 | 2016-03-30 | 杨晓林 | A kind of edible oil comprising molecular marker and its preparation method and application |
| CN103798414A (en) * | 2012-11-13 | 2014-05-21 | 杨晓林 | Edible oil containing molecular markers as well as preparation method and application thereof |
| CN103134921A (en) * | 2012-12-27 | 2013-06-05 | 北京智云达科技有限公司 | Illegal cooking oil colloidal gold fast measuring card |
| CN104198639A (en) * | 2014-09-09 | 2014-12-10 | 中国石油化工股份有限公司 | Quantitative analysis method for micromolecular organic acids in fluid extracted from oil field |
| CN105424856A (en) * | 2015-11-25 | 2016-03-23 | 四川北方硝化棉股份有限公司 | Method for detecting acyl content in cellulose acetate butyrate |
| CN107192767A (en) * | 2016-03-15 | 2017-09-22 | 中国水产科学研究院 | The method that isotopic dilution gaschromatographic mass spectrometry determines eugenol in aquatic products |
| CN108732274A (en) * | 2018-06-20 | 2018-11-02 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of assessment method of edible oil and fat |
| CN113866304A (en) * | 2021-09-28 | 2021-12-31 | 浙江大学 | Method for measuring content of volatile fatty acid in rumen fluid of ruminant |
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