CN103439366A - Method for detecting repeated heating of edible vegetable oil by use of electronic nose - Google Patents
Method for detecting repeated heating of edible vegetable oil by use of electronic nose Download PDFInfo
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- CN103439366A CN103439366A CN2013103724119A CN201310372411A CN103439366A CN 103439366 A CN103439366 A CN 103439366A CN 2013103724119 A CN2013103724119 A CN 2013103724119A CN 201310372411 A CN201310372411 A CN 201310372411A CN 103439366 A CN103439366 A CN 103439366A
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Abstract
The invention provides a method for detecting repeated heating of edible vegetable oil by use of an electronic nose. The method includes the steps of placing the edible vegetable oil into a sealing sample bottle to prepare a headspace sample; sucking headspace gas in the sample bottle with a sampling needle, injecting the headspace gas into a sampling port of the electronic nose and detecting the headspace gas by use of a provided gas sensor array, wherein the gas sensor array comprises a chlorine/fluorine/nitrogen/oxygen/ammonia compound sensor, an ethanol sensor, a hydrogen sulfide sensor, a methane/propane/butane sensor, a hydrocarbon compound sensor, a methylbenzene/xylene sensor and a combustion product sensor; and collecting numerical values acquired by the gas sensors, performing data analysis and constructing a model, thereby distinguishing whether the edible vegetable oil suffers from repeated heating. The sample treatment method is simple without any organic solvent, sample using amount is little, and rapid and nondestructive detection can be realized. Besides, the overall information of the sample is provided, and therefore, the method can be used for effectively distinguishing whether the edible vegetable oil suffers from repeated heating. The simple and rapid analysis and detection method is high in reliability.
Description
Technical field
The invention belongs to the food inspection technical field, relate to a kind of method that detection by electronic nose edible vegetable oil heats repeatedly.
Background technology
Fried food is important food composition, comprises Chinese deep-fried twisted dough sticks, oil cake, fried fried dough twist, and the chips in foreign fast food, chrips, fried chicken wing etc.The making of fried food be unable to do without the high-temperature heating of edible vegetable oil.In order to produce fried food as much as possible, edible oil can remain the condition of high temperature in a long time.On the other hand, for cost-saving, the edible oil after heating is recovered usually, and in the production run of next fried food, continues edible.This has just caused the heating repeatedly of edible vegetable oil.
The edible vegetable oil of this heating repeatedly is huge for the harm of human health, especially can increase the risk of suffering from hypertension, high fat of blood, coronary heart disease and cancer.The edible vegetable oil of making for fried food is in heating process repeatedly, can be hydrolyzed, the series of chemical such as oxidation, polymerization, decomposition, produces the objectionable impuritiess such as benzopyrene, acrylamide, is not suitable for the consumer edible.Need to set up and repeatedly heat the edible vegetable oil detection method.
The existing detection method indexs such as the color by analyzing edible soybean oil, viscosity, surface tension, saponification rate, acid value, peroxide value, component is basically differentiated, although above-mentioned detection method is reliable, method of operating is comparatively complicated, need the sample size time more, that detect also longer.Therefore, in order to ensure consumer's physical and mental health, set up the quick and lossless detection method that repeatedly heats edible vegetable oil, become the important composition of China's food security art research and development.
Summary of the invention
The objective of the invention is to set up a kind of edible vegetable oil detection method that repeatedly heats, make fast, edible vegetable oil is heated in Non-Destructive Testing repeatedly becomes possibility.The specific embodiment of the invention step is as follows:
1. headspace sample preparation: take 2 g edible vegetable oil to be measured and be placed in 10 ml sample bottles, and seal with the silica gel dottle pin.Be placed in 6 METAL HEATING PROCESS casees, set temperature is 34 ℃, each example reaction 15 min.
2. testing conditions: Sai Kesaisi QL-10 oil-free air pump and QL-Z1500 zero level air generator produce without the oil drying air as carrier gas, flow velocity 150 ml/min, volume injected 2 ml, be 2 min detection time, lag time 12 min, utilize the Electronic Nose sample introduction needle to obtain the head space gas inject Electronic Nose injection port in sample bottle.
The Electronic Nose model is FOX4000(Alpha MOS, France), contain 18 sensors.Sensor type comprises chlorine/fluorine/nitrogen/oxygen/ammoniate sensor, ethanol sensor, hydrogen sulfide sensor, methane/propane/butane sensor, hydrocarbon sensor, toluene/dimethylbenzene sensor, products of combustion sensor.
3. data analysis: adopt the PCA statistical method to carry out the efficiency analysis of Electronic Nose experimental technique.Utilize sensor array to be detected, sensor array is comprised of 3 matrix chambers, each matrix chamber comprises 6 sensors, amount to 18 sensors, collect the numerical value that the Electronic Nose sensor gathers, carry out principal component analysis (PCA), it is threshold value that the validity of principal component analysis (PCA) be take PC1 and PC2 contribution rate 90%, if contribution rate is less than this threshold value, shows that needs revise the detected parameters of Electronic Nose.
Take edible soybean oil as example, if the PC1 in pca model and PC2 contribution rate are greater than 90%, mean that the detection by electronic nose method of setting up is good, can meet the analysis requirement.If the contribution rate of pca model, lower than 90%, means to need to improve the testing conditions of Electronic Nose.
4. result judgement: adopt the SQC method to set up Quality Control Model, for judging that whether edible vegetable oil is through heating repeatedly.In SQC controls illustraton of model, horizontal ordinate means the detection number of times of sample, and ordinate means the parasang of odor characteristics value, usings 0 mean value as the sample odor characteristics.There is no the both sides of the sample distribution of heating at mean value.Two parallel lines are arranged in the SQC model, be respectively upper control limit and lower control limit, the sample of odor characteristics value in upper lower control limit is the edible vegetable oil that there is no heating, otherwise is considered as because repeatedly heating the sample of abnormal quality.
Be to utilize statistical quality control analysis model whether to carry out edible vegetable oil through the judgement of heating repeatedly, take that there is no the edible vegetable oil of heating be quality control standard, exceed belonging to of critical field and produce the edible vegetable oil of mass change because repeatedly heat.
Another object of the present invention is to provide the described edible vegetable oil detection method that repeatedly heats in the application detected in repeatedly heating edible vegetable oil.
Electronic Nose Technology is a kind of simple, fast novel analyzing detecting method.The technology of the present invention compared with prior art, its sample treatment is simple, without any need for organic solvent, sample use amount few (2 g), can realize that quick nondestructive detects, and the Global Information of sampling, can effectively judge that whether edible vegetable oil is through heating repeatedly.
The accompanying drawing explanation
Fig. 1: the process flow diagram of edible vegetable oil is heated in the Electronic Nose Technology analysis repeatedly.
Fig. 2: the Electronic Nose pca model detects the gold dragon fish board soybean oil after heating repeatedly.
Fig. 3: the good fortune after the detection of Electronic Nose pca model is heated repeatedly is the board soybean oil near the house.
Fig. 4: the favour that the Electronic Nose pca model detects after heating repeatedly should board (Wal-Mart) soybean oil.
Fig. 5: Electronic Nose SQC model detects the gold dragon fish board soybean oil after heating repeatedly.
Fig. 6: the good fortune after the detection of Electronic Nose SQC model is heated repeatedly is the board soybean oil near the house.
Fig. 7: the favour that Electronic Nose SQC model detects after heating repeatedly should board (Wal-Mart) soybean oil.
Fig. 8: Electronic Nose SQC model detects the many power board sunflower oil after heating repeatedly.
Fig. 9: Electronic Nose SQC model detects the gold dragon fish board rapeseed oil after heating repeatedly.
Figure 10: the good fortune after the detection of Electronic Nose SQC model is heated repeatedly is board corn oil near the house.
Figure 11: Electronic Nose SQC model detects the gold dragon fish board peanut oil after heating repeatedly.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further elaborated, but embodiment does not limit the scope of the invention.
Embodiment 1: the edible soybean oil heated through is repeatedly divided in the detection by electronic nose technical area;
Preparation is the edible vegetable oil of heating repeatedly: the edible vegetable oil of common brand on market, utilize " frying pattern " (300 W) of electromagnetic oven, and heat 60 min, after being cooled to room temperature, then carry out the next round heating, heating amounts to 5 times repeatedly.Sample after heating is placed in vial, in the room temperature sealing, keeps in Dark Place.3 repetitions are set, and each repeats 500 g edible vegetable oils.
Prepare the human consumption soybean oil samples of heating repeatedly, carry out Electronic Nose Technology with reference to the process flow diagram shown in Fig. 1 and detect the soybean oil of heating repeatedly.Accurately weighing 2 g samples, put into 10 ml sample bottles, and, at 34 ℃ of reaction 15 min, extract 2 ml head space gases, injects the injection port of Electronic Nose, and the data that produce after 18 sensors detect are carried out analysis by different statistical methods.In pca model shown in Fig. 2, the contribution rate of PC1 and PC2 has surpassed 99%, shows that the detection by electronic nose system of setting up can meet the research needs.Simultaneously, pca model can find that the favour of different number of times heating should present different distributions for board (Wal-Mart) soybean oil, and the soybean oil of heating presents by positive axis and distributes to negative semiaxis along the PC1 axle according to heating times repeatedly.Good fortune PC1 and the PC2 contribution rate of the soybean oil of brand and Jin Long fish products board has near the house all surpassed 90% threshold value (Fig. 3-4), shows that the detection method of setting up can carry out further research.
In order to judge that whether human consumption soybean has through heating repeatedly, we carry out Quality Control Analysis by building the SQC model.Result shows do not have the contrast soybean oil of heating mainly to be distributed in the gray area in the SQC model, and namely the odor characteristics value, in upper lower control limit, belongs to normal specimens; Soybean oil odor characteristics value through heating is distributed in beyond control limit, and this presents the trend (Fig. 5) increased gradually apart from the increase along with heating times.The SQC model also can be for distinguishing the different heating number of times to the impact (Fig. 6-7) of brand and Jin Long fish products board soybean oil near the house.
Embodiment 2: Electronic Nose Technology is distinguished sunflower oil, rapeseed oil, corn oil and the peanut oil of heating repeatedly.
Utilize the Electronic Nose Technology detection system of setting up, also studied and repeatedly heated the impact on other edible vegetable oil.Result shows, peanut oil, sunflower oil and corn wet goods edible oil are after repeatedly heating, the sample quality changes, and shows as the odor characteristics value beyond the upper lower control limit of SQC Quality Control Model, and the normal edible oil of heating is not in controlling limit with interior (Fig. 8-10).Such as, many power board sunflower oil through heating is different from the edible oil that there is no heating, along with the increase of heating times repeatedly, sample is more and more obvious with the difference that contrasts sunflower oil, shows as the sunflower oil odor characteristics value that repeatedly heats after 5 times apart from the standard of bound (Fig. 8) farthest.Except many power board sunflower oil, Electronic Nose SQC model also can effectively be distinguished gold dragon fish board rapeseed oil (Fig. 9) through heating repeatedly, good fortune board corn oil (Figure 10) and golden imperial fish board peanut oil (Figure 11) near the house.
Claims (4)
1. the method that detection by electronic nose edible vegetable oil heats repeatedly, is characterized in that, by following steps, realizes:
(1) headspace sample preparation: get 2 g edible vegetable oil to be measured and be placed in 10 ml sample bottles, and, with the sealing of silica gel dottle pin, then sample bottle is placed in to 6 METAL HEATING PROCESS casees, set temperature is 34 ℃, each example reaction 15 min;
(2) testing conditions: Sai Kesaisi QL-10 oil-free air pump and QL-Z1500 zero level air generator produce without the oil drying air as carrier gas, flow velocity 150 ml/min, volume injected 2 ml, be 2 min detection time, lag time 12 min, utilize the Electronic Nose sample introduction needle to obtain the head space gas inject Electronic Nose injection port in sample bottle;
(3) data analysis: utilize sensor array to be detected, sensor array is comprised of 3 matrix chambers, each matrix chamber comprises 6 sensors, amount to 18 sensors, collect the numerical value that the Electronic Nose sensor gathers, carry out principal component analysis (PCA), it is threshold value that the validity of principal component analysis (PCA) be take PC1 and PC2 contribution rate 90%, if contribution rate is less than this threshold value, shows that needs revise the detected parameters of Electronic Nose;
(4) result judgement: adopt statistical quality control analysis method to set up Quality Control Model, for judging that whether edible vegetable oil is through heating repeatedly, in the statistical quality control analysis, control in illustraton of model, horizontal ordinate means the detection number of times of sample, ordinate means the parasang of odor characteristics value, using 0 mean value as the sample odor characteristics, there is no the both sides of the sample distribution of heating at mean value, two parallel lines are arranged in statistical quality control analysis model, be respectively upper control limit and lower control limit, the sample of odor characteristics value in upper lower control limit be not for there is no the edible vegetable oil of heating, otherwise be considered as because repeatedly heating the sample of abnormal quality.
2. the method that a kind of detection by electronic nose edible vegetable oil according to claim 1 heats repeatedly, it is characterized in that, step (2) Electronic Nose model used is FOX4000, contain 18 sensors, sensor type comprises chlorine/fluorine/nitrogen/oxygen/ammoniate sensor, ethanol sensor, hydrogen sulfide sensor, methane/propane/butane sensor, hydrocarbon sensor, toluene/dimethylbenzene sensor, products of combustion sensor.
3. the method that a kind of detection by electronic nose edible vegetable oil according to claim 1 heats repeatedly, it is characterized in that, step (4) is to utilize statistical quality control analysis model whether to carry out edible vegetable oil through the judgement of heating repeatedly, take that there is no the edible vegetable oil of heating be quality control standard, exceed belonging to of critical field and produce the edible vegetable oil of mass change because repeatedly heat.
4. method claimed in claim 1 is in the application detected in repeatedly heating edible vegetable oil.
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| CN103743786A (en) * | 2013-12-19 | 2014-04-23 | 中安高科检测科技（北京）有限公司 | Method for preparing gas sensor array for detecting mutton |
| CN104849435A (en) * | 2015-05-29 | 2015-08-19 | 宁波大学 | Rapid identification method for crude oil, crude oil degradation product, finished product oil and analog |
| CN105527391A (en) * | 2015-12-31 | 2016-04-27 | 浙江海洋学院 | Electric-nose-analysis-based determination method of tuna oil corruption degree in storage process |
| CN105628883A (en) * | 2015-12-31 | 2016-06-01 | 浙江海洋学院 | Ethyl ester type fish oil quality evaluation method based on electronic nose analysis |
| CN107271619A (en) * | 2017-06-21 | 2017-10-20 | 无锡中科恒源信息科技有限公司 | The online test method of harmful substance, apparatus and system in edible oil heating process |
| CN110879258A (en) * | 2019-10-31 | 2020-03-13 | 天津科技大学 | Method for predicting relation between food material processing and flavor quality of food material based on electronic nose and application of method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104849435A (en) * | 2015-05-29 | 2015-08-19 | 宁波大学 | Rapid identification method for crude oil, crude oil degradation product, finished product oil and analog |
| CN105527391A (en) * | 2015-12-31 | 2016-04-27 | 浙江海洋学院 | Electric-nose-analysis-based determination method of tuna oil corruption degree in storage process |
| CN105628883A (en) * | 2015-12-31 | 2016-06-01 | 浙江海洋学院 | Ethyl ester type fish oil quality evaluation method based on electronic nose analysis |
| CN107271619A (en) * | 2017-06-21 | 2017-10-20 | 无锡中科恒源信息科技有限公司 | The online test method of harmful substance, apparatus and system in edible oil heating process |
| CN110879258A (en) * | 2019-10-31 | 2020-03-13 | 天津科技大学 | Method for predicting relation between food material processing and flavor quality of food material based on electronic nose and application of method |
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Application publication date: 20131211 |