CN106442776B - A method of measurement acetyl content - Google Patents
A method of measurement acetyl content Download PDFInfo
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- CN106442776B CN106442776B CN201610822718.8A CN201610822718A CN106442776B CN 106442776 B CN106442776 B CN 106442776B CN 201610822718 A CN201610822718 A CN 201610822718A CN 106442776 B CN106442776 B CN 106442776B
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Abstract
The invention discloses a kind of methods for measuring acetyl content, and in particular to a method of combine full volatilization headspace gas chromatography to measure acetyl content using chemical conversion.It the steps include: (1) preparing standard solution；(2) standard curve is established；(3) sample treatment；(4) analysis detection is carried out using HS GC；(5) result calculates.The beneficial effect of this method is, adopts the content for measuring acetyl group with the aforedescribed process, has many advantages, such as that convenient and efficient, accuracy is high, and is suitble to sample batch detection.
Description
Technical field
The invention belongs to analysis detection fields, and in particular to a method of measurement acetyl content.
Background technique
Acetyl group is the acyl function being made of methyl and carbonyl, is a kind of important function base.It is present in
In many kinds of substance, such as plant fiber material, converted starch and chitosan etc..Institute's acetyl-containing is in slurrying in plant fiber material
With will form organic acid in pre-hydrolysis process, to will affect the consumption of alkali in pulping process and the utilization of subsequent pre-hydrolyzed solution.
And the number of acetyl content also has important influence for the property of substance in the substances such as converted starch, chitosan.Vinegar
The property of Esterification converted starch is mainly influenced by acetyl content, and as acetyl content increases, viscosity is reduced, transparency
It increases, gelatinization point reduces, and dehydration and retrogradation reduce.Thus can according to acetyl content number, selection be best suited for institute
The acetic acid esterified converted starch of food is produced, to reach optimal application effect.Therefore, Accurate Determining acetate content for
Matter utilization or material mass control all have significance.
The method of measurement acetyl content mainly has biological enzyme and titration at present, and wherein titration application is more wide
It is general.Titration is that acetyl group is hydrolyzed to form to acetic acid, acetic acid neutralization titration measurement content is then distilled out, to acquire second
The content of acyl group, the method measurement result is more accurate, but needs to distill, cumbersome time-consuming.Therefore it establishes a kind of easy, fast
Speed, the method for Accurate Determining acetyl content are particularly necessary.
Summary of the invention
It is an object of the invention to overcome drawback present in the method for measurement acetyl content at present, a kind of measurement is provided
The method of acetyl content.Measuring principle of the invention is under the action of p-methyl benzenesulfonic acid ethanol solution, and acetyl group is converted
For ethyl acetate, the ethyl acetate amount then generated using full volatilization Headspace-Gas Chromatography Analysis measurement, so that sample be calculated
The content of middle acetyl group.It may be implemented quickly to measure according to this method, easy to operate and easy grasp, analysis result accuracy
Height has certain practicability, is suitble to batch detection.
The present invention is achieved by the following technical solutions.
A method of measurement acetyl content, this method combine full volatilization head space-gas phase color using chemical conversion technology
Spectrometry measures the content of acetyl group, specifically includes the following steps:
(1) it prepares ethyl acetate standard solution: accurately measuring suitable ethyl acetate in volumetric flask, add dehydrated alcohol fixed
Hold to volumetric flask scale and obtains ethyl acetate standard solution；
(2) it establishes standard curve: using head-space sampler, the second of different volumes is separately added into multiple headspace sample bottles
Acetoacetic ester standard solution, and sealed sample bottle, are then placed on sample stage, then carry out HS GC detection,
A standard curve can be obtained between gained ethyl acetate signal peak area and ethyl acetate additional amount；
(3) sample treatment: sample to be tested is placed in a reaction flask, and suitable p-methyl benzenesulfonic acid and anhydrous is added in bottle
Then ethyl alcohol seals, be placed in water-bath and handled, and reaction terminates to use dehydrated alcohol constant volume after cooling in ice bath, to
Measurement；
(4) analysis detection: it is accurate to measure appropriate treated solution to be measured, it is added with head-space sampler to head space sample
In product bottle, and headspace sample bottle is sealed, be placed on sample stage, then carried out HS GC detection, record sample
The ethyl acetate chromatographic peak area of product；
(5) result calculates: peak area obtained by step (4) being compared with step (2) standard curve, is obtained by calculation
The content of acetyl group in sample.
It advanced optimizes, the concentration of ethyl acetate standard solution described in step (1) is 0.1~20.0g/L.
It advanced optimizes, the ethyl acetate standard solution volume of addition described in step (2) is 0~45 μ L.
It advanced optimizes, the mass ratio of the sample to be tested of addition described in step (3), p-methyl benzenesulfonic acid and dehydrated alcohol
It is 1: 10: 30~1: 100: 300.
Advanced optimize, in step (3) the oil bath pot temperature of placing response bottle be 60~120 DEG C, the reaction time be 5~
120min。
It advanced optimizes, the operating condition of head-space sampler in step (2) and (4) are as follows: sample injector furnace temp 60
~115 DEG C；0.5~the 8.0min of equilibration time of ml headspace bottle in an oven.
It advanced optimizes, gas-chromatography operating condition in step (2) and (4) are as follows: column temperature is 25-49 DEG C；Carrier gas is helium
Gas, flow velocity are 3.0~5.0mL/min；Detector is flame ionization detector (FID), and detector temperature is 200~250
℃。
It advanced optimizes, suitable sample to be tested is taken described in step (4), volume is 5~40 μ L.
It advanced optimizes, the calculation formula of acetyl content described in step (5) are as follows:
In formula, C is the content of ethyl acetate in sample after the processing obtained by standard curve；V is at step (3) sample
Overall solution volume after managing constant volume；M is sample to be tested oven dry weight；43 be the molecular weight of acetyl group；88 dividing for ethyl acetate
Son amount.
It advanced optimizes, the method for said determination acetyl content specifically comprises the following steps:
(1) it prepares ethyl acetate standard solution: accurately measuring suitable ethyl acetate in volumetric flask, add dehydrated alcohol fixed
Hold to volumetric flask scale and obtains ethyl acetate standard solution.
(2) establish standard curve: be separately added into a series of headspace sample bottle 0~45 μ L concentration be 0.1~
The ethyl acetate standard solution of 20.0g/L, and sealed sample bottle, are then placed on sample stage, then carry out head space-gas
The detection of phase chromatography, can obtain a standard curve between gained ethyl acetate signal peak area and ethyl acetate additional amount.
(3) sample treatment: sample to be tested, p-methyl benzenesulfonic acid and the anhydrous second for being 1: 10: 30~1: 100: 300 by mass ratio
Alcohol sequentially adds in reaction flask, then seals, and is placed in water-bath, and 5~120min, reaction knot are reacted at 60~120 DEG C
Dehydrated alcohol constant volume is used after beam is cooling in ice bath, it is to be determined.
(4) analysis detection: 5~40 μ L treated solution to be measured is accurately measured, it is added with micro-sampling pin to top
In empty sample bottle, and sealed sample bottle, it is placed on sample stage, then carries out HS GC detection, record sample
The ethyl acetate chromatographic peak area of product.
(5) result calculates: peak area obtained by step (4) being compared with step (2) standard curve, is obtained by calculation
The content of acetyl group in sample.
Compared with prior art, the invention has the advantages that and technical effect:
(1) this method is easy to operate, and specificity is strong；
(2) accuracy of this method is good, and sensitivity is higher；
(3) the continuous mode time is short；
(4) strong antijamming capability；
(5) it is suitble to batch detection.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.The invention is not limited to following implementation.
The examples are only for explaining the invention, is not intended to limit the present invention, and should belong to the present invention for the simple change for being related to of the invention
Protection scope.
The calculation formula of acetyl content in following embodiment are as follows:
In formula, C is the content of ethyl acetate in sample after the processing obtained by standard curve；V is at step (3) sample
Overall solution volume after managing constant volume；M is sample to be tested oven dry weight；43 be the molecular weight of acetyl group；88 dividing for ethyl acetate
Son amount.
The measurement of acetyl content in 1 plant fiber material of embodiment
(1) prepare ethyl acetate standard solution: the accurate ethyl acetate for measuring 1.000g adds dehydrated alcohol in volumetric flask
It is settled to 100mL and obtains ethyl acetate standard solution.
(2) establish standard curve: using head-space sampler, be separately added into 0 in multiple headspace sample bottles, 5,10,15,
20, the ethyl acetate standard solution of 25,30,40 μ L, and sealed sample bottle, are then placed on sample stage, then carry out
HS GC detection, can obtain a standard song between gained ethyl acetate signal peak area and ethyl acetate additional amount
Line.
(3) sample treatment: 0.200g sample to be tested (plant fiber material) is placed in a reaction flask, and 5g is added in bottle
P-methyl benzenesulfonic acid and 20g dehydrated alcohol, then seal, are placed in water-bath, and 30min is reacted at 100 DEG C, and reaction terminates
It is settled to 50mL with dehydrated alcohol after cooling in ice bath, it is to be determined.
(4) analysis detection: it is accurate to measure 30 μ L treated solution to be measured, it is added with micro-sampling pin to head space sample
In product bottle, and sealed sample bottle, it is placed on sample stage, then carries out HS GC detection, record sample
Ethyl acetate chromatographic peak area.The operating condition of head-space sampler described above are as follows: 85 DEG C of furnace temp；Headspace sample bottle exists
Equilibration time 4.5min in baking oven, gas-chromatography operating condition are as follows: column temperature is 40 DEG C；Carrier gas is helium, flow velocity 4.0mL/
min；Detector is flame ionization detector, and detector temperature is 225 DEG C.
(5) result determines: peak area obtained by step (4) being compared with step (2) standard curve, is obtained by calculation
The content of acetyl group in sample.The results are shown in Table 1 for determination data.
Table 1
The measurement of acetyl content in 2 converted starch of embodiment
(1) prepare ethyl acetate standard solution: the accurate ethyl acetate for measuring 2.000g adds dehydrated alcohol in volumetric flask
It is settled to 100mL and obtains ethyl acetate standard solution.
(2) establish standard curve: using head-space sampler, be separately added into 0 in multiple headspace sample bottles, 5,10,15,
20, the ethyl acetate standard solution of 25,30,40 μ L, and sealed sample bottle, are then placed on sample stage, then carry out
HS GC detection, can obtain a standard song between gained ethyl acetate signal peak area and ethyl acetate additional amount
Line.
(3) sample treatment: 0.100g sample to be tested (converted starch) is placed in a reaction flask, and 10g pairs is added in bottle
Toluenesulfonic acid and 50g dehydrated alcohol, then seal, are placed in water-bath, and 20min is reacted at 100 DEG C, and reaction terminates in ice
It is settled to 50mL with dehydrated alcohol after cooling in bath, it is to be determined.
(4) analysis detection: it is accurate to measure 30 μ L treated solution to be measured, it is added with sample injector to headspace sample bottle
In, and sealed sample bottle, it is placed on sample stage, then carries out HS GC detection, record the acetic acid of sample
Ethyl ester chromatographic peak area.The operating condition of head-space sampler described above are as follows: 115 DEG C of furnace temp；Headspace sample bottle is drying
Equilibration time 8.0min in case, gas-chromatography operating condition are as follows: column temperature is 49 DEG C；Carrier gas is helium, flow velocity 5.0mL/
min；Detector is flame ionization detector, and detector temperature is 250 DEG C.
Table 2
(5) result determines: peak area obtained by step (4) being compared with step (2) standard curve, is obtained by calculation
The content of acetyl group in sample.The results are shown in Table 2 for determination data.
Claims (5)
1. a kind of method for measuring acetyl content, which is characterized in that this method combines full volatilization top using chemical conversion technology
Sky-gas chromatography measurement acetyl group content, specifically includes the following steps:
(1) prepare ethyl acetate standard solution: the accurate ethyl acetate that measures adds dehydrated alcohol to be settled to volumetric flask in volumetric flask
Scale obtains ethyl acetate standard solution；
(2) it establishes standard curve: using head-space sampler, the acetic acid second of different volumes is separately added into multiple headspace sample bottles
Ester standard solution, and headspace sample bottle is sealed, it is then placed on sample stage, then carry out HS GC detection, gained second
A standard curve can be obtained between acetoacetic ester signal peak area and ethyl acetate additional amount；
(3) sample treatment: sample to be tested is placed in a reaction flask, and p-methyl benzenesulfonic acid and dehydrated alcohol are added in bottle, then
Sealing, is placed in water-bath and is handled, cooling again with dehydrated alcohol constant volume in ice bath after reaction, to be determined；It is described
The mass ratio of sample to be tested, p-methyl benzenesulfonic acid and dehydrated alcohol is 1: 10: 30 ~ 1: 100: 300；The water-bath pot temperature of placing response bottle
Degree is 60 ~ 120 DEG C, and the reaction time is 5 ~ 120min；
(4) analysis detection: the solution to be measured that accurately measures that step (3) treated, then be added with head-space sampler to headspace sample
In bottle, and headspace sample bottle is sealed, be placed on sample stage, then carried out HS GC detection, record the second of sample
Acetoacetic ester chromatographic peak area；
(5) result calculates: peak area obtained by step (4) being compared with step (2) standard curve, sample is obtained by calculation
The content of middle acetyl group；The calculation formula of the content of the acetyl group are as follows:
In formula, C is the content of ethyl acetate in sample after the processing obtained by standard curve；V is that step (3) sample treatment is fixed
Overall solution volume after appearance；M is sample to be tested oven dry weight；43 be the molecular weight of acetyl group；88 be the molecular weight of ethyl acetate；
Gas-chromatography operating condition used in step (2) and step (4) are as follows: column temperature is 25-49 DEG C；Carrier gas is helium, flow velocity
For 3.0 ~ 5.0 mL/min；Detector is flame ionization detector, and detector temperature is 200 ~ 250 DEG C.
2. a kind of method for measuring acetyl content according to claim 1, it is characterised in that: second described in step (1)
The concentration of acetoacetic ester standard solution is 0.1 ~ 20.0 g/L.
3. a kind of method for measuring acetyl content according to claim 1, it is characterised in that: second described in step (2)
The volume that acetoacetic ester standard solution is added is 0 ~ 45 μ L.
4. a kind of method for measuring acetyl content according to claim 1, it is characterised in that: step (2) and step
(4) operating condition of the head-space sampler described in are as follows: sample injector furnace temp is 60 ~ 115 DEG C；Headspace sample bottle is in baking oven
In equilibration time be 0.5 ~ 8.0 min.
5. it is according to claim 1 it is a kind of measure acetyl content method, it is characterised in that: described in step (4) to
The volume for surveying solution is 5 ~ 40 μ L.
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|---|---|---|---|---|
| CN104655775A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for measuring 3-acetyl-2, 5-dimethyl thiophene in edible flavor and fragrance |
| CN104655753A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for determining 3-acetyl-2, 5-thioxene in food additive |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104655775A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for measuring 3-acetyl-2, 5-dimethyl thiophene in edible flavor and fragrance |
| CN104655753A (en) * | 2015-02-10 | 2015-05-27 | 广西中烟工业有限责任公司 | Method for determining 3-acetyl-2, 5-thioxene in food additive |
Non-Patent Citations (3)
| Title |
|---|
| Analysis of acetyl groups in biological materials by gas chromatography;G.R.Shepherd 等;《Analytical Biochemistry》;19681231;第26卷;325-340 |
| Analysis of the Acetyl Groups in Ovine Luteinizing Hormone by Gas Chromatography;Darrell N. Ward 等;《Biochemistry》;19641031;第3卷(第10期);1575-1577 |
| 气相色谱法检测增香大米中的2_乙酰基吡啶;冯永巍 等;《粮食与饲料工业》;20141231(第7期);60-62 |
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