CN106442776A - Method for measuring acetyl content - Google Patents
Method for measuring acetyl content Download PDFInfo
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- CN106442776A CN106442776A CN201610822718.8A CN201610822718A CN106442776A CN 106442776 A CN106442776 A CN 106442776A CN 201610822718 A CN201610822718 A CN 201610822718A CN 106442776 A CN106442776 A CN 106442776A
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Abstract
The invention discloses a method for measuring acetyl content, and particularly relates to a method for measuring acetyl content by chemical conversion combined with all volatile headspace gas chromatography. The method includes the steps that 1, a standard solution is prepared; 2, a standard curve is set up; 3, samples are processed; 4, headspace-gas chromatography is used for analysis detection; 5, results are calculated. The method has the advantages of being convenient, fast, high in accuracy and suitable for detecting samples in batches when used for measuring acetyl content.
Description
Technical field
The invention belongs to analysis detection field is and in particular to a kind of method of mensure acetyl content.
Background technology
Acetyl group is an acyl function being made up 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, modified starch and shitosan etc..In plant fiber material, institute's acetyl-containing is in slurrying
With can form organic acid in pre-hydrolysis process, thus can affect alkali in pulping process consume and follow-up pre-hydrolyzed solution utilization.
And the number of acetyl content also has important impact for the property of material in the materials such as modified starch, shitosan.Vinegar
The property of Esterification modified starch is mainly affected by acetyl content, raises with acetyl content, and viscosity reduces, transparency
Raise, gelatinization point reduces, dehydration and retrogradation reduce.Thus can according to acetyl content number, select be best suited for institute
Produce the acetic acid esterified modified starch of food, to reaching optimal application effect.Therefore, Accurate Determining acetate content for
Matter utilization or material mass control are respectively provided with significance.
The method measuring acetyl content at present mainly has biological enzyme and titrimetry, and wherein titrimetry application is more wide
General.Titrimetry is that acetyl group is hydrolyzed to form acetic acid, then distills out acetic acid neutralization titration and measures content, thus trying to achieve second
The content of acyl group, this method measurement result is more accurate, but needs to distill, and its complex operation is time-consuming.Hence set up a kind of easy, fast
Fast, Accurate Determining acetyl content method is particularly necessary.
Content of the invention
It is an object of the invention to the drawbacks of overcome existing for the method measuring acetyl content at present, provide a kind of mensure
The method of acetyl content.The measuring principle of the present invention is that acetyl group is converted in the presence of p-methyl benzenesulfonic acid ethanol solution
For ethyl acetate, then measure, using the full Headspace-Gas Chromatography Analysis that volatilize, the ethyl acetate amount producing, thus being calculated sample
The content of middle acetyl group.Can realize quickly measuring according to the method, simple to operate and easy grasp, its analysis result accuracy
Height, has certain practicality, suitable batch detection.
The present invention is achieved by the following technical solutions.
A kind of method measuring acetyl content, the method utilizes chemical conversion technology to combine the full head space-gas phase color that volatilizees
Spectrometry measures the content of acetyl group, specifically includes following steps：
(1) prepare ethyl acetate standard solution：Accurately measure appropriate ethyl acetate in volumetric flask, plus dehydrated alcohol is fixed
Hold and obtain ethyl acetate standard solution to volumetric flask scale；
(2) Criterion curve：Using head-space sampler, multiple headspace sample bottles are separately added into the second of different volumes
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 addition；
(3) sample treatment：Testing sample is placed in reaction bulb, and adds appropriate p-methyl benzenesulfonic acid and anhydrous in bottle
Ethanol, then seals, and is positioned in water-bath and is processed, and reaction terminates in ice bath and uses dehydrated alcohol constant volume after cooling, treats
Measure；
(4) analysis detection：Accurately measure the solution to be measured after appropriate process, it is added to head space sample with head-space sampler
In product bottle, and seal headspace sample bottle, be placed on sample stage, then carry out HS GC detection, record sample
The ethyl acetate chromatographic peak area of product；
(5) result calculates：Step (4) gained peak area is compared with step (2) standard curve, by being calculated
The content of acetyl group in sample.
Optimize further, the concentration of ethyl acetate standard solution described in step (1) is 0.1～20.0g/L.
Optimize further, the ethyl acetate standard solution volume adding described in step (2) is 0～45 μ L.
Optimize further, the mass ratio of the testing sample, p-methyl benzenesulfonic acid and dehydrated alcohol that add described in step (3)
For 1: 10: 30～1: 100: 300.
Optimize further, in step (3) the oil bath pot temperature of placing response bottle be 60～120 DEG C, the response time be 5～
120min.
Optimize further, in step (2) and (4), the operating condition of head-space sampler is：Injector furnace temp 60
～115 DEG C；Ml headspace bottle equilibration time 0.5～8.0min in an oven.
Optimize further, in step (2) and (4), gas chromatogram operating condition is：Column temperature is 25-49 DEG C；Carrier gas is helium
Gas, its flow velocity is 3.0～5.0mL/min；Detector is flame ionization detector (FID), and detector temperature is 200～250
℃.
Optimize further, described in step (4), take appropriate testing sample, its volume is 5～40 μ L.
Optimize further, described in step (5), the computing formula of acetyl content is：
In formula, C is the content of ethyl acetate in sample after the process being obtained by standard curve；V is at step (3) sample
Overall solution volume after reason constant volume；M is testing sample oven dry weight；43 is the molecular weight of acetyl group；88 is dividing of ethyl acetate
Son amount.
Optimize further, the method for said determination acetyl content specifically includes following steps：
(1) prepare ethyl acetate standard solution：Accurately measure appropriate ethyl acetate in volumetric flask, plus dehydrated alcohol is fixed
Hold and obtain ethyl acetate standard solution to volumetric flask scale.
(2) Criterion curve：A series of headspace sample bottle is separately added into 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
Phase chromatograph detects, can obtain a standard curve between gained ethyl acetate signal peak area and ethyl acetate addition.
(3) sample treatment：Testing sample, p-methyl benzenesulfonic acid and the anhydrous second that mass ratio is 1: 10: 30～1: 100: 300
Alcohol sequentially adds in reaction bulb, then seals, and is positioned in water-bath, reacts 5～120min, reaction knot at 60～120 DEG C
Bundle uses dehydrated alcohol constant volume after cooling down in ice bath, to be determined.
(4) analysis detection：Accurately measure the solution to be measured after 5～40 μ L are processed, it is added to top with micro-sampling pin
In empty sample bottle, and sealed sample bottle, it is placed on sample stage, then carry out HS GC detection, record sample
The ethyl acetate chromatographic peak area of product.
(5) result calculates：Step (4) gained peak area is compared with step (2) standard curve, by being calculated
The content of acetyl group in sample.
Compared with prior art, the invention has the advantages that and technique effect：
(1) the method is easy and simple to handle, and specificity is strong；
(2) accuracy of the method is good, and sensitivity is higher；
(3) the continuous mode time is short；
(4) strong antijamming capability；
(5) it is suitable for batch detection.
Specific embodiment
With reference to embodiment, the present invention is described in further detail.The invention is not limited in implementation below.
Embodiment is only used for explaining the present invention, and the unrestricted present invention, the present invention all should be belonged to for the simple change being related to the present invention
Protection domain.
In following examples, the computing formula of acetyl content is：
In formula, C is the content of ethyl acetate in sample after the process being obtained by standard curve；V is at step (3) sample
Overall solution volume after reason constant volume；M is testing sample oven dry weight；43 is the molecular weight of acetyl group；88 is dividing of ethyl acetate
Son amount.
The mensure of acetyl content in embodiment 1 plant fiber material
(1) prepare ethyl acetate standard solution：The ethyl acetate accurately measuring 1.000g is in volumetric flask, plus dehydrated alcohol
It is settled to 100mL and obtain ethyl acetate standard solution.
(2) Criterion curve：Using head-space sampler, multiple headspace sample bottles are separately added into 0,5,10,15,
20th, the ethyl acetate standard solution of 25,30,40 μ L, and sealed sample bottle, is then placed on sample stage, then carries out
HS GC detects, can obtain a standard song between gained ethyl acetate signal peak area and ethyl acetate addition
Line.
(3) sample treatment：0.200g testing sample (plant fiber material) is placed in reaction bulb, and adds 5g in bottle
P-methyl benzenesulfonic acid and 20g dehydrated alcohol, then seal, and are positioned in water-bath, react 30min at 100 DEG C, and reaction terminates in
It is settled to 50mL with dehydrated alcohol after cooling down in ice bath, to be determined.
(4) analysis detection：Accurately measure the solution to be measured after 30 μ L are processed, it is added to head space sample with micro-sampling pin
In product bottle, and sealed sample bottle, it is placed on sample stage, then carry out HS GC detection, record sample
Ethyl acetate chromatographic peak area.The operating condition of the above head-space sampler is：85 DEG C of furnace temp；Headspace sample bottle exists
Equilibration time 4.5min in baking oven, gas chromatogram operating condition is：Column temperature is 40 DEG C；Carrier gas is helium, and flow velocity is 4.0mL/
min；Detector is flame ionization detector, and detector temperature is 225 DEG C.
(5) result determines：Step (4) gained peak area is compared with step (2) standard curve, by being calculated
The content of acetyl group in sample.Determination data result is as shown in table 1.
Table 1
The mensure of acetyl content in embodiment 2 modified starch
(1) prepare ethyl acetate standard solution：The ethyl acetate accurately measuring 2.000g is in volumetric flask, plus dehydrated alcohol
It is settled to 100mL and obtain ethyl acetate standard solution.
(2) Criterion curve：Using head-space sampler, multiple headspace sample bottles are separately added into 0,5,10,15,
20th, the ethyl acetate standard solution of 25,30,40 μ L, and sealed sample bottle, is then placed on sample stage, then carries out
HS GC detects, can obtain a standard song between gained ethyl acetate signal peak area and ethyl acetate addition
Line.
(3) sample treatment：0.100g testing sample (modified starch) is placed in reaction bulb, and adds 10g pair in bottle
Toluenesulfonic acid and 50g dehydrated alcohol, then seal, and are positioned in water-bath, react 20min at 100 DEG C, and reaction terminates in ice
It is settled to 50mL with dehydrated alcohol after cooling down in bath, to be determined.
(4) analysis detection：Accurately measure the solution to be measured after 30 μ L are processed, it is added to headspace sample bottle with injector
In, and sealed sample bottle, it is placed on sample stage, then carry out HS GC detection, record the acetic acid of sample
Ethyl ester chromatographic peak area.The operating condition of the above head-space sampler is：115 DEG C of furnace temp；Headspace sample bottle is drying
Equilibration time 8.0min in case, gas chromatogram operating condition is：Column temperature is 49 DEG C；Carrier gas is helium, and flow velocity is 5.0mL/
min；Detector is flame ionization detector, and detector temperature is 250 DEG C.
Table 2
(5) result determines：Step (4) gained peak area is compared with step (2) standard curve, by being calculated
The content of acetyl group in sample.Determination data result is as shown in table 2.
Claims (9)
1. a kind of method measuring acetyl content is it is characterised in that the method utilizes chemical conversion technology to combine full volatilization top
Sky-gas chromatography measures the content of acetyl group, specifically includes following steps：
（1）Prepare ethyl acetate standard solution：Accurately measure ethyl acetate in volumetric flask, plus dehydrated alcohol is settled to volumetric flask
Scale obtains ethyl acetate standard solution；
（2）Criterion curve：Using head-space sampler, multiple headspace sample bottles are separately added into the acetic acid second of different volumes
Ester standard solution, and seal headspace sample bottle, 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 addition；
（3）Sample treatment：Testing sample is placed in reaction bulb, and adds p-methyl benzenesulfonic acid and dehydrated alcohol in bottle, then
Sealing, is positioned in water-bath and is processed, and reaction terminates to cool down in rear ice bath uses dehydrated alcohol constant volume again, to be determined；
（4）Analysis detection：Accurately measure step（3）Solution to be measured after process, then added to headspace sample with head-space sampler
In bottle, and seal headspace sample bottle, be positioned on sample stage, then carry out HS GC detection, record the second of sample
Acetoacetic ester chromatographic peak area；
（5）Result calculates：By step（4）Gained peak area and step（2）Standard curve is compared, by being calculated sample
The content of middle acetyl group.
2. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（1）Described in second
The concentration of acetoacetic ester standard solution is 0.1 ~ 20.0 g/L.
3. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（2）Described in second
The volume that acetoacetic ester standard solution adds is 0 ~ 45 μ L.
4. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（3）Described in treat
The mass ratio of test sample product, p-methyl benzenesulfonic acid and dehydrated alcohol is 1: 10: 30 ~ 1: 100: 300.
5. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（3）Middle placement is anti-
The water-bath pot temperature answering bottle is 60 ~ 120 DEG C, and the response time is 5 ~ 120min.
6. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（2）With step
（4）Described in the operating condition of head-space sampler be：Injector furnace temp is 60 ~ 115 DEG C；Headspace sample bottle is in baking oven
In equilibration time be 0.5 ~ 8.0 min.
7. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（2）And step
（4）In gas chromatogram operating condition used be：Column temperature is 25-49 DEG C；Carrier gas is helium, and flow velocity is 3.0 ~ 5.0 mL/min；
Detector is flame ionization detector, and detector temperature is 200 ~ 250 DEG C.
8. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（5）Described in second
The computing formula of the content of acyl group is：
In formula, C is the content of ethyl acetate in sample after the process being obtained by standard curve；V is step（3）Sample treatment is fixed
Overall solution volume after appearance；M is testing sample oven dry weight；43 is the molecular weight of acetyl group；88 is the molecular weight of ethyl acetate.
9. according to claim 1 a kind of measure acetyl content method it is characterised in that：Step（4）Described in treat
The volume surveying solution is 5 ~ 40 μ L.
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| CN201610822718.8A CN106442776B (en) | 2016-09-13 | 2016-09-13 | A method of measurement acetyl content |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107389837A (en) * | 2017-07-20 | 2017-11-24 | 山东钢铁集团日照有限公司 | A kind of device of air extraction volatile organic matter |
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| 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 |
| 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 |
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- 2016-09-13 CN CN201610822718.8A patent/CN106442776B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| DARRELL N. WARD 等: "Analysis of the Acetyl Groups in Ovine Luteinizing Hormone by Gas Chromatography", 《BIOCHEMISTRY》 * |
| G.R.SHEPHERD 等: "Analysis of acetyl groups in biological materials by gas chromatography", 《ANALYTICAL BIOCHEMISTRY》 * |
| 冯永巍 等: "气相色谱法检测增香大米中的2_乙酰基吡啶", 《粮食与饲料工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107389837A (en) * | 2017-07-20 | 2017-11-24 | 山东钢铁集团日照有限公司 | A kind of device of air extraction volatile organic matter |
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