CN104777262A - Method for authenticating three broccoliflorets varieties by gas chromatography - Google Patents
Method for authenticating three broccoliflorets varieties by gas chromatography Download PDFInfo
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- CN104777262A CN104777262A CN201510179941.0A CN201510179941A CN104777262A CN 104777262 A CN104777262 A CN 104777262A CN 201510179941 A CN201510179941 A CN 201510179941A CN 104777262 A CN104777262 A CN 104777262A
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Abstract
The invention discloses a method for authenticating three broccoliflorets varieties by gas chromatography. The method comprises the following steps: obtaining authentication samples through acetonitrile extraction and acetone volume metering, then authenticating by the gas chromatography with an authentication chromatographic column of DB-1701, then, determining the nature by authenticating the ratio between the retention time and the peak area of each target peak of a sample, wherein Youxiu and Xique varieties have four target peaks respectively, Yanxiu variety only has two target peaks, the ratio of the peal areas of the third target peak and the first target peak of the Youxiu variety is 1.9-3.2, the ratio of the peal areas of the third target peak and the first target peak of the Xique variety is 1.0-18.2, the retention time of the three varieties is stable, the ratio of the peal areas of the third target peak and the first target peak of the Youxiu variety and the ratio of the peal areas of the third target peak and the first target peak of the Xique variety have a great difference and obvious distinction, and therefore, the authentication is accurate. According to the method disclosed by the invention, simplicity can be realized, learning is easy, authentication is convenient, and the method is especially suitable for basic scientific research departments in broccoliflorets production places.
Description
Technical field
The present invention relates to the discriminating of Broccoliflorets kind, be specifically related to the method differentiating three Broccoliflorets kinds by vapor-phase chromatography.
Background technology
Broccoliflorets belongs to crucifer, has another name called broccoli or broccoli, is Common Vegetables crop.What Ningbo area was planted is scorching elegant, outstanding and magpie three kinds, these three kinds are difficult to distinguish from morphology, molecules authentication technique requires higher, the scientific research department of general county, town level does not have ability to distinguish, therefore provide a kind of Broccoliflorets variety discriminating method simple, easy to learn to the scientific research department of basic unit in the Broccoliflorets place of production, there is actual application value.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method that vapor-phase chromatography differentiates three Broccoliflorets kinds, and the method is simple, easy to learn, has and differentiates convenience, accurately advantage.
The present invention solves the problems of the technologies described above adopted technical scheme: the method differentiating three Broccoliflorets kinds by vapor-phase chromatography, and its step is as follows:
A, take 25.0g Broccoliflorets sample and be placed in reagent bottle, add acetonitrile 50.0ml, with refiner with 15500 rpm homogenate 2min, leave standstill and extract 30min, filter, filtrate being poured into is added with in the centrifuge tube of 4g sodium chloride, and vibration 1min, shakes up; Centrifuge tube is with the centrifugal 6min of 4000 rpm, and stratification, draws upper organic phase 10.0ml in the test tube of band plug, and test tube blows in the Nitrogen evaporator of 80 DEG C of water-baths to be done near, is settled to 5.0ml, obtains differentiating sample with acetone;
B, discriminating sample vapor-phase chromatography are differentiated, GC conditions: carrier gas is high pure nitrogen, flow 30ml/min; Hydrogen flowing quantity is 75ml/min, air mass flow 110ml/min; Pressure 9.95psi before post, current constant mode, tail nitrogen blowing; Injector temperature 220 DEG C, detector temperature 25 DEG C; Adopt Splitless injecting samples mode, sample size 1 μ l, sample introduction 0.85min post-purge; DB-1701 chromatographic column, column temperature program: initial temperature 100 DEG C, is warming up to 200 DEG C with 40 DEG C/min, then is warming up to 210 DEG C with 2 DEG C/min, is then warming up to 240 DEG C with 30 DEG C/min, and retain 4min and all flow out to sample;
C, qualitative with the ratio of the retention time and peak area of differentiating the target peak of sample, the wherein outstanding target peak having four identical retention times with magpie kind, scorching elegant kind only has the target peak of two identical retention times, namely No. 3 target peaks and No. 4 target peaks are only had, the retention time of four target peaks is respectively: No. 1 target peak is 2.434 ~ 2.435min, No. 2 target peaks are 2.549 ~ 2.550min, and No. 3 target peaks are 3.939 ~ 3.941min, and No. 4 target peaks are 5.487 ~ 5.489min; No. 3 target peaks of outstanding kind are 1.9 ~ 3.2 with the ratio of the peak area of No. 1 target peak, and No. 3 target peaks of magpie kind are 11.0 ~ 18.2 with the ratio of the peak area of No. 1 target peak.
Compared with prior art, the invention has the advantages that the method differentiating three Broccoliflorets kinds by vapor-phase chromatography, extracted by acetonitrile, acetone constant volume, obtain differentiating sample, differentiate by vapor-phase chromatography again, discriminating chromatographic column is DB-1701, then qualitative with the ratio of the retention time and peak area of differentiating the target peak of sample, as outstanding and magpie kind have four target peaks, scorching elegant kind only has two objects peak, No. 3 target peaks of outstanding kind are 1.9 ~ 3.2 with the ratio of the peak area of No. 1 target peak, No. 3 target peaks of magpie kind are 11.0 ~ 18.2 with the ratio of the peak area of No. 1 target peak, the retention time of these three kinds is stablized, can qualitatively be Broccoliflorets, two objects peak is scorching elegant kind, as for outstanding large with the ratio difference of the peak area of No. 1 target peak with No. 3 target peaks that are magpie kind, difference obviously, therefore differentiate accurately, method of the present invention is simple, easy to learn, it is convenient to differentiate, be particularly useful for the scientific research department of basic unit in the cauliflower place of production.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
The Broccoliflorets sample 25.0g Broccoliflorets sample that Hu Shan food market, Cixi Gu Tang street is purchased is placed in reagent bottle, add acetonitrile 50.0ml, with refiner with 15500 rpm (r/min) homogenate 2min, leave standstill and extract 30min, filter, filtrate being poured into is added with in the centrifuge tube of 4g sodium chloride, and vibration 1min, shakes up; Centrifuge tube is with the centrifugal 6min of 4000 rpm, and stratification, draws upper organic phase 10.0ml in the test tube of band plug, and test tube blows in the Nitrogen evaporator of 80 DEG C of water-baths to be done near, is settled to 5.0ml, obtains differentiating sample with acetone; Differentiate that sample vapor-phase chromatography is differentiated, GC conditions: carrier gas is high pure nitrogen, flow 30ml/min; Hydrogen flowing quantity is 75ml/min, air mass flow 110ml/min; Pressure 9.95psi before post, current constant mode, tail nitrogen blowing; Injector temperature 220 DEG C, detector temperature 25 DEG C; Adopt Splitless injecting samples mode, sample size 1 μ l, sample introduction 0.85min post-purge; DB-1701 chromatographic column, column temperature program: initial temperature 100 DEG C, is warming up to 200 DEG C with 40 DEG C/min, then is warming up to 210 DEG C with 2 DEG C/min, is then warming up to 240 DEG C with 30 DEG C/min, and retain 4min and all flow out to sample; Qualitative with the ratio of the retention time (appearance time) and peak area of differentiating the target peak of sample, solvent acetone is internal standard compound, the appearance time of acetone is 0.747 ~ 0.750min, the appearance time obtaining No. 1 target peak is 2.434min, the appearance time of No. 2 target peaks is 2.549min, the appearance time of No. 3 target peaks is 3.939min, the appearance time of No. 4 target peaks is 5.487min, and No. 3 target peaks are 2.5 with the ratio of the peak area of No. 1 target peak, illustrate that this Broccoliflorets is outstanding kind, can confirm further by HP-5 chromatographic column.
Embodiment 2
Substantially the same manner as Example 1, difference is Broccoliflorets sample is growing vegetables family, Chen Jia village, Cixi City Zhang Qi town Wu Hong China, the appearance time obtaining No. 1 target peak is 2.435min, the appearance time of No. 2 target peaks is 2.549min, the appearance time of No. 3 target peaks is 3.941min, the appearance time of No. 4 target peaks is 5.489min, and No. 3 target peaks are 3.1 with the ratio of the peak area of No. 1 target peak, illustrate that this Broccoliflorets is outstanding kind.
Embodiment 3
Substantially the same manner as Example 1, difference is Broccoliflorets sample is that the leaf treasure spring sowing of Jiangkou village, Cixi City Zhou Xiang town three is planted, the appearance time obtaining No. 1 target peak is 2.435min, the appearance time of No. 2 target peaks is 2.550min, the appearance time of No. 3 target peaks is 3.940min, the appearance time of No. 4 target peaks is 5.488min, and No. 3 target peaks are 2.0 with the ratio of the peak area of No. 1 target peak, illustrate that this Broccoliflorets is outstanding kind.
Embodiment 4
Substantially the same manner as Example 1, difference is Broccoliflorets sample is the Cen Qian health plantation of haze mountain village, Creek Pu town, Zhenhai District, the appearance time only obtaining No. 3 target peaks is 3.939min, and the appearance time of No. 4 target peaks is 5.488min, illustrates that this Broccoliflorets is scorching elegant kind.
Embodiment 5
Substantially the same manner as Example 1, difference is Broccoliflorets sample is that Yue Lin street, Fenghua City Yuan Guohai plants, and the appearance time obtaining No. 3 target peaks is 3.941min, and the appearance time of No. 4 target peaks is 5.487min, illustrates that this Broccoliflorets is scorching elegant kind.
Embodiment 6
Substantially the same manner as Example 1, difference is Broccoliflorets sample is that water cloud Pu village, Cixi City Xiao Lin town Hu grace conservation is planted, the appearance time obtaining No. 1 target peak is 2.435min, the appearance time of No. 2 target peaks is 2.550min, the appearance time of No. 3 target peaks is 3.940min, the appearance time of No. 4 target peaks is 5.488min, and No. 3 target peaks are 14.5 with the ratio of the peak area of No. 1 target peak, illustrate that this Broccoliflorets is magpie kind.
Embodiment 7
Substantially the same manner as Example 1, difference is Broccoliflorets sample is that Cixi City Xiao Lin town Lian Ming village Fang Zhencai plants, the appearance time obtaining No. 1 target peak is 2.434min, the appearance time of No. 2 target peaks is 2.549min, the appearance time of No. 3 target peaks is 3.941min, the appearance time of No. 4 target peaks is 5.489min, and No. 3 target peaks are 18.0 with the ratio of the peak area of No. 1 target peak, illustrate that this Broccoliflorets is magpie kind.
Embodiment 8
Substantially the same manner as Example 1, difference is Broccoliflorets sample is the free and unfettered curb village scholar Jiang ripple plantation of Cixi City Xiao Lin town, the appearance time obtaining No. 1 target peak is 2.435min, the appearance time of No. 2 target peaks is 2.550min, the appearance time of No. 3 target peaks is 3.939min, the appearance time of No. 4 target peaks is 5.487min, and No. 3 target peaks are 11.2 with the ratio of the peak area of No. 1 target peak, illustrate that this Broccoliflorets is magpie kind.
We show through repeatedly repeatedly studying: 3 Broccoliflorets kinds of Ningbo City, " scorching elegant " Broccoliflorets kind only has No. 3 peaks, No. 4 peaks, there is no No. 1 peak, No. 2 peaks, outstanding, magpie 4 target peaks have identical retention time, retention time is very stable, and within the certain scope of all each leisure of ratio at No. 1 peak, No. 3 peak/, the ratio of outstanding kind No. 3 peaks and No. 1 peak area is between 1.9 ~ 3.2; The ratio of magpie kind No. 3 peaks and No. 1 peak area is between 11.0 ~ 18.2, and difference obviously.
Claims (1)
1. differentiate the method for three Broccoliflorets kinds by vapor-phase chromatography, it is characterized in that step is as follows:
A, take 25.0g Broccoliflorets sample and be placed in reagent bottle, add acetonitrile 50.0ml, with refiner with 15500 rpm homogenate 2min, leave standstill and extract 30min, filter, filtrate being poured into is added with in the centrifuge tube of 4g sodium chloride, and vibration 1min, shakes up; Centrifuge tube is with the centrifugal 6min of 4000 rpm, and stratification, draws upper organic phase 10.0ml in the test tube of band plug, and test tube blows in the Nitrogen evaporator of 80 DEG C of water-baths to be done near, is settled to 5.0ml, obtains differentiating sample with acetone;
B, discriminating sample vapor-phase chromatography are differentiated, GC conditions: carrier gas is high pure nitrogen, flow 30ml/min; Hydrogen flowing quantity is 75ml/min, air mass flow 110ml/min; Pressure 9.95psi before post, current constant mode, tail nitrogen blowing; Injector temperature 220 DEG C, detector temperature 25 DEG C; Adopt Splitless injecting samples mode, sample size 1 μ l, sample introduction 0.85min post-purge; DB-1701 chromatographic column, column temperature program: initial temperature 100 DEG C, is warming up to 200 DEG C with 40 DEG C/min, then is warming up to 210 DEG C with 2 DEG C/min, is then warming up to 240 DEG C with 30 DEG C/min, and retain 4min and all flow out to sample;
C, qualitative with the ratio of the retention time and peak area of differentiating the target peak of sample, the wherein outstanding target peak having four identical retention times with magpie kind, scorching elegant kind only has the target peak of two identical retention times, namely No. 3 target peaks and No. 4 target peaks are only had, the retention time of four target peaks is respectively: No. 1 target peak is 2.434 ~ 2.435 min, No. 2 target peaks are 2.549 ~ 2.550 min, and No. 3 target peaks are 3.939 ~ 3.941 min, and No. 4 target peaks are 5.487 ~ 5.489 min; No. 3 target peaks of outstanding kind are 1.9 ~ 3.2 with the ratio of the peak area of No. 1 target peak, and No. 3 target peaks of magpie kind are 11.0 ~ 18.2 with the ratio of the peak area of No. 1 target peak.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823842A (en) * | 2016-03-29 | 2016-08-03 | 慈溪市农业监测中心 | Method for distinguishing three varieties of common head cabbages |
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2015
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Patent Citations (4)
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| JPH0739400A (en) * | 1993-08-02 | 1995-02-10 | Sumitomo Chem Co Ltd | Method for discriminating plant variety using oligonucleotide |
| CN102735685A (en) * | 2012-06-15 | 2012-10-17 | 南京众合生物科技有限责任公司 | Quintuplet identification method for quality detection of Cordyceps sinensis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823842A (en) * | 2016-03-29 | 2016-08-03 | 慈溪市农业监测中心 | Method for distinguishing three varieties of common head cabbages |
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