CN101487833B - Method for recognizing natural apple essence - Google Patents

Method for recognizing natural apple essence Download PDF

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Publication number
CN101487833B
CN101487833B CN2009100788305A CN200910078830A CN101487833B CN 101487833 B CN101487833 B CN 101487833B CN 2009100788305 A CN2009100788305 A CN 2009100788305A CN 200910078830 A CN200910078830 A CN 200910078830A CN 101487833 B CN101487833 B CN 101487833B
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sample
natural apple
head space
apple essence
electronic nose
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CN101487833A (en
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倪元颖
陈晓明
李景明
马丽艳
石宝霞
刘远方
郑如力
张晓华
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China Agricultural University
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China Agricultural University
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Abstract

The invention discloses a method for identifying the natural apple essences using sensor-type electronic noses to achieve the identification of the natural apple essences. The inventive method is characterized by simple pretreatment of samples, no use of organic solvents in the whole experiment, no pollution, fast detection speed, and high identification precision, and the inventive method has simple procedure, and convenient operation, and is suitable for large-scale popularization. The invention is conductive for perfecting the detection project of the natural apple essences, and mastering the variation of different natural apple essences, and has significant economic value for the production and sale fields of the natural apple essences.

Description

A kind of method of discerning natural apple essence
Technical field
The present invention relates to a kind of method of discerning natural apple essence.
Background technology
Natural apple essence is to obtain in the apple deep-processing process, and owing to deriving from nature, containing hundreds of kind fragrance component, its strong and distinctive apple delicate fragrance is that any compound essence does not all replace.Flavoring apple essence is the very rare adjuvants of industry such as food, cosmetic, and especially wherein distinctive organic substance is a chemical industry material very in short supply, so flavoring apple essence more and more is subjected to the favor of international market.In recent years, natural apple essence outlet increased year by year, and requirement of client is also more and more stricter, and the essence content is being understood under the not enough condition, needed during sale send the client sample earlier, and detect and confirm by the client, be very passive.In today that essence turnout and export volume enlarge day by day, how to improve the test item of flavoring apple essence and the situation of change of grasping different times and different cultivars flavoring apple essence, seeming becomes more and more important.
At present the quality of essence and flavoring agent is mainly by some physical indexs such as refraction index, relative density, acidity value, fugitive constituent total amounts and manually smell fragrant these two links and control.The former can only reflect some characteristic of essence and flavoring agent on the whole; And the latter with the nose sense as identification facility, be subjected to the influence of factors such as subjective consciousness, environment and individual difference, can not accurately reflect the inherent quality and the fluctuation thereof of essence.And above-mentioned operated in accordance with conventional methods complexity, the analytic process required time is long.
Electronic Nose (Electronic Nose), claim artificial olfactory analysis system (Artificial Olfactory) again, be analysis, identification and the detection technique of a kind of novelty of growing up the nineties in 20th century, the artificial intelligence system of forming by sensor-based system and automatic mode recognition system of discerning at various smells, its the similar people's of principle of work nose is so be referred to as " Electronic Nose ".Electronic Nose has merged the current new results in active fields such as materialogy, electronic signal, applied mathematics, sensing and computer science the most, once producing great attention and the common attention that just has been subjected to external scientific circles.
Summary of the invention
The invention provides a kind of method of discerning the natural apple essence aroma quality.
The method of identification natural apple essence aroma quality provided by the invention is to treat the right flavoring apple essence of observation with the sensor type Electronic Nose to discern.
In the described method, the head space injection parameters of Electronic Nose can be set to: volume injected 200-300 μ l, injection speed 200-300 μ l/s, 60-80 ℃ of entry needle temperature.The head space injection parameters of Electronic Nose specifically can be set to: volume injected 200-250 μ l, injection speed 200-250 μ l/s, 60-70 ℃ of entry needle temperature.The head space injection parameters of Electronic Nose specifically also can be set to: volume injected 250-300 μ l, injection speed 250-300 μ l/s, 70-80 ℃ of entry needle temperature.
In the described method, the static headspace gas sample size of natural apple essence to be measured can be 100 μ l-1ml, as can be 100 μ l-250 μ l or 250 μ l-1ml.
In the described method, the head space of Electronic Nose produces parameter and can be set to: it is 25-80 ℃ that head space produces temperature, head space generation time 100-200s, and the sample agitation speed is 100-300rpm.Described head space produces temperature and specifically can be 60-80 ℃.
In the described method, the head space of Electronic Nose produces parameter and specifically can be set to: it is 60-70 ℃ that head space produces temperature, head space generation time 100-150s, and the sample agitation speed is 100-200rpm.The head space of Electronic Nose produces parameter and specifically also can be set to: it is 70-80 ℃ that head space produces temperature, head space generation time 150-200s, and the sample agitation speed is 200-300rpm.
The present invention is applied to the sensor type Electronic Nose identification of natural apple essence first, and by a large amount of tests, has obtained best parameter setting scope, and when adopting the parameter in this scope, discrimination index is very high.Take the inventive method, sample pre-treatments is simple; Whole experiment is not utilized organic solvent, and is pollution-free; Detection speed was fast, and the corresponding steps of static headspace gas generation step required time and gas chromatography is approaching, but the analysis recognition time of each sample only needs about 3 minutes, much smaller than 0.5-1 hour of gas chromatography; The recognition accuracy height; The inventive method step is simple, and is easy to operate, is convenient to large-scale promotion application.The present invention helps to improve the test item of flavoring apple essence, helps to grasp the situation of change of different quality flavoring apple essences, has great economic worth for the production and selling field of natural apple essence.
Embodiment
Following embodiment is convenient to understand better the present invention, but does not limit the present invention.Experimental technique among the following embodiment if no special instructions, is conventional method.Reagent among the following embodiment if no special instructions, is can buy from routine biochemistry reagent and obtains.
Used sensor type Electronic Nose is available from French Alpha MOS instrument company in following examples, and model is FOX4000.Natural apple essence sample used in following examples is as follows:
The natural apple essence sample standard deviation is purchased in northern An Deli fruit juice company limited by shares, has the sample of 36 different production batch of three aroma quality grades.Wherein the natural apple essence of each grade comprises the sample of 12 different production batch.
The recognition capability of Electronic Nose to sample represented in following discrimination index (Discrimination Index is called for short DI), calculated by following formula:
DI=[1-(the gross space areas of the summation of each cohort spatial area/all cohorts of containing)] * 100.
In principal component analysis (PCA) (PCA) collection of illustrative plates of sample, if when not superposeing between the cohort, DI be on the occasion of, when between the cohort stack being arranged, DI is a negative value, shows between the sample and can not distinguish fully.The maximal value of DI is 100, and DI just shows effective differentiation between 80-100, and the DI value is big more, and it is good more to distinguish.
The identification of embodiment 1, natural apple essence
Each sample detects respectively, and is specific as follows:
1 μ l natural apple essence is put into sample bottle (the sample bottle specification is 10ml), be positioned over the static headspace gas generating means, it is 25 ℃ that head space produces temperature, and the head space generation time is 100s, and the sample agitation speed is 100rpm.Extract static headspace gas with the Electronic Nose sample introduction needle then, be expelled in the Electronic Nose injection port, the static headspace gas sample size is 100 μ l, the static headspace gas injection parameters: volume injected 200 μ l, injection speed 200 μ l/s, 60 ℃ of entry needle temperature.
Each sample carries out revision test 6 times.
Through principal component analysis (PCA) (PCA) software that Electronic Nose carries the data of being obtained are analyzed.Analysis result shows: the accumulation variance contribution ratio of first principal component (PC1) and Second principal component, (PC2) is 92.342%, 2.587%, is 94 by the two-dimensional map discrimination index (DI) that PC1 (X-axis)-PC2 (Y-axis) is constituted.Wherein the accumulation variance contribution ratio sum of PC1 and PC2 is 94.929%, and greater than 85%, this explanation PC1 and PC2 have comprised the very big quantity of information of sample, can reflect the Global Information of sample.Discrimination index (DI) is 94, and the sample of this explanation different brackets can well be distinguished, and recognition result conforms to actual, and recognition result is correct.In 6 repeated experiments, the discrimination index unanimity, repeatability is fabulous.Adopt the sample of method identification different aromas quality of the present invention, it is short to analyze recognition time, and sample pre-treatments is simple, does not also utilize organic solvent in the experimentation.
The identification of embodiment 2, natural apple essence
Each sample detects respectively, and is specific as follows:
1 μ l natural apple essence is put into sample bottle (the sample bottle specification is 10ml), be positioned over the static headspace gas generating means, it is 70 ℃ that head space produces temperature, and the head space generation time is 150s, and the sample agitation speed is 200rpm.Extract static headspace gas with the Electronic Nose sample introduction needle then, be expelled in the Electronic Nose injection port, the static headspace gas sample size is 250 μ l, the static headspace gas injection parameters: volume injected 250 μ l, injection speed 250 μ l/s, 70 ℃ of entry needle temperature.
Each sample carries out revision test 6 times.
Through principal component analysis (PCA) (PCA) software that Electronic Nose carries the data of being obtained are analyzed.Analysis result shows: the accumulation variance contribution ratio of first principal component (PC1) and Second principal component, (PC2) is 97.382%, 2.521%, is 98 by the two-dimensional map discrimination index (DI) that PC1 (X-axis)-PC2 (Y-axis) is constituted.Wherein the accumulation variance contribution ratio sum of PC1 and PC2 is 99.903%, and greater than 85%, this explanation PC1 and PC2 have comprised the very big quantity of information of sample, can reflect the Global Information of sample.Discrimination index (DI) is 98, and the sample of this explanation different brackets can well be distinguished, and recognition result conforms to actual, and recognition result is correct.In 6 repeated experiments, the discrimination index unanimity, repeatability is fabulous.Adopt the sample of method identification different aromas quality of the present invention, it is short to analyze recognition time, and sample pre-treatments is simple, does not also utilize organic solvent in the experimentation.
The identification of embodiment 3, natural apple essence
Each sample detects respectively, and is specific as follows:
1 μ l natural apple essence is put into sample bottle (the sample bottle specification is 10ml), be positioned over the static headspace gas generating means, it is 80 ℃ that head space produces temperature, and the head space generation time is 200s, and the sample agitation speed is 300rpm.Extract static headspace gas with the Electronic Nose sample introduction needle then, be expelled in the Electronic Nose injection port, the static headspace gas sample size is 1ml, the static headspace gas injection parameters: volume injected 300 μ l, injection speed 300 μ l/s, 80 ℃ of entry needle temperature.
Each sample carries out revision test 6 times.
Through principal component analysis (PCA) (PCA) software that Electronic Nose carries the data of being obtained are analyzed.Analysis result shows: the accumulation variance contribution ratio of first principal component (PC1) and Second principal component, (PC2) is 90.196%, 3.343%, is 92 by the two-dimensional map discrimination index (DI) that PC1 (X-axis)-PC2 (Y-axis) is constituted.Wherein the accumulation variance contribution ratio sum of PC1 and PC2 is 93.539%, and greater than 85%, this explanation PC1 and PC2 have comprised the very big quantity of information of sample, can reflect the Global Information of sample.Discrimination index (DI) is 92, and the sample of this explanation different aromas quality can well be distinguished, and recognition result conforms to actual, and recognition result is correct.In 6 repeated experiments, the discrimination index unanimity, repeatability is fabulous.Adopt the sample of method identification different aromas quality of the present invention, it is short to analyze recognition time, and sample pre-treatments is simple, does not also utilize organic solvent in the experimentation.

Claims (2)

1. a method of discerning natural apple essence is to treat the right flavoring apple essence of observation with the sensor type Electronic Nose to discern;
The head space injection parameters of Electronic Nose is: volume injected 200-300 μ l, injection speed 200-300 μ l/s, 60-80 ℃ of entry needle temperature;
The head space of Electronic Nose produces parameter: head space produces 25-80 ℃ of temperature, head space generation time 100-200s, and the sample agitation speed is 100-300rpm;
The static headspace gas sample size of natural apple essence to be measured is 100 μ l-1ml.
2. the method for claim 1 is characterized in that: in the described method, it is 60-80 ℃ that head space produces temperature.
CN2009100788305A 2009-03-03 2009-03-03 Method for recognizing natural apple essence Expired - Fee Related CN101487833B (en)

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CN104897729A (en) * 2015-06-04 2015-09-09 安徽农业大学 Sorting method of storage time of melon slice tea by using electronic nose

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1381721A (en) * 2002-06-04 2002-11-27 复旦大学 Portable intelligent electronic nose and its preparing process

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1381721A (en) * 2002-06-04 2002-11-27 复旦大学 Portable intelligent electronic nose and its preparing process

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
陈晓明.天然苹果香精香气质量综合评价模型的建立及电子鼻的应用研究.《中国农业大学硕士学位论文》.2006,1-70. *
陈晓明等.电子鼻在天然苹果香精检测中的应用.《食品科学》.2007,第28卷(第3期),261页. *
陈晓明等.电子鼻在食品工业中的应用研究进展.《传感器与微系统》.2006,第25卷(第4期), *

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