CN104391049B - Detection method for residual quantity of xanthan gum microscale solvent - Google Patents
Detection method for residual quantity of xanthan gum microscale solvent Download PDFInfo
- Publication number
- CN104391049B CN104391049B CN201410507809.3A CN201410507809A CN104391049B CN 104391049 B CN104391049 B CN 104391049B CN 201410507809 A CN201410507809 A CN 201410507809A CN 104391049 B CN104391049 B CN 104391049B
- Authority
- CN
- China
- Prior art keywords
- standard solution
- sample
- xanthan gum
- ethanol
- propyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A disclosed detection method for residual quantity of a xanthan gum microscale solvent comprises the following main steps: (1) preparing a standard solution of n-propanol; (2) preparing a standard solution of ethanol; (3) preparing a mixed standard solution; (4) preparing a sample solution; (5) utilizing gas chromatograph for detection and recording the chromatogram; and (6) calculating the residual ethanol content in the xanthan gum sample. The method for detecting alcohol in xanthan gum is designed through a large amount of experiments and research based on the different characteristics of xanthan gum compared with other food and food additives. The method is simple, practicable and high in accuracy, is capable of the content of a microscale solvent with the detection limit of 1 ppm, and is extremely suitable for detection by xanthan gum production manufacturers and xanthan gum user laboratories, thereby enabling the food-grade xanthan gum to reach domestic and international food safety requirements during usage.
Description
Technical field
The present invention relates to the detection method of xanthan gum trace solvent residual quantity, belongs to the detection of the solvent residual amount of xanthan gum
Method field.
Background technology
Xanthan gum, as a kind of nontoxic, harmless colloid, is to collect at present thickening, suspension in the world, emulsifying, be stable in one
Body. best performance biogum more.Which is widely used in food and chemical industry.Current domestic food level xanthan gum manufacturing enterprise
The overwhelming majority is extracted as solvent with edible ethanol, and in its final products, ethanol has certain residual, but European Union and U.S.
There is strict demand in state to alcohol content in food and food additive, there is presently no minimal residue in being specifically designed for xanthan gum molten
The detection method of agent alcohol content.According to the xanthan gum characteristic different from other food and food additive, by substantial amounts of reality
Test and research, the method for having made alcohol content in detection xanthan gum, the method are simple and easy to do, and accuracy is high, can verify that
Output is limited to the trace solvent content of 1ppm, is especially suitable for the detection of xanthan gum manufacturer and xanthan gum customer laboratory.
The content of the invention
It is an object of the invention to provide a kind of detection method of xanthan gum trace solvent residual quantity, so that food stage xanthan
Glue can reach the requirement of internal and international upper food safety in use；The know-why of the present invention is by sample xanthan peptization
Micro-content organism ethanol is reclaimed by Yu Shuizhong using distillation condensation method, detects the content of ethanol using gas chromatograph.
The detection method of xanthan gum trace solvent residual quantity, is characterized in that the detection method step is as follows：
(1) prepare the standard solution of normal propyl alcohol：Concentration is prepared with chromatographically pure anhydrous normal propyl alcohol and redistilled water is
The normal propyl alcohol standard solution of 1mg/ml, it is standby；
(2) prepare the standard solution of ethanol：It is 1mg/ml that concentration is prepared with chromatographically pure dehydrated alcohol and redistilled water
Ethanol standard solution, it is standby；
(3) prepare mixed standard solution：Using the ethanol standard solution of the normal propyl alcohol standard solution and 1mg/ml of 1mg/ml
It is and redistilled water prepares mixed standard solution of the concentration for ethanol 0.04mg/ml and normal propyl alcohol 0.04mg/ml, standby；
(4) preparation of sample solution：First the xanthan gum sample of quality w=4g is placed in the round-bottomed flask of 500ml, then
The redistilled water for accurately measuring 200ml is added in this round-bottomed flask, then round-bottomed flask is fixed on agitator and is vibrated
1h, adds the defoamer of about 2ml, this round-bottomed flask is connected to distillation condensing units again then, is steamed after sample dissolving
Evaporate, distillation amount is V1 (about 100ml), and distillation amount V2 (about 95ml) for taking distillate is put in the volumetric flask of 100ml, finally
The normal propyl alcohol standard solution of 4ml is added, and finally 100ml (constant volume is V3=100ml) is settled to redistilled water, is sample
Product solution, it is standby：
(5) detected using gas chromatograph and record chromatogram：The temperature for controlling gas chromatographic column is 55 DEG C, injection port temperature
It is 200 DEG C to spend for 180 DEG C, checker temperature, and carrier gas during inspection is nitrogen；The mixed standard solution of 1ul is initially injected, is surveyed
Fixed, record chromatogram, determines peak height and peak width and calculates peak area；The sample solution of 1ul is then injected into, is measured, is recorded
Chromatogram, determines peak height and peak width and calculates peak area；
(6) calculate the ethanol content remained in xanthan gum sample：In measure, the ethanol and normal propyl alcohol of sample solution is corresponding
The ethanol peak area of coefficient f1=sample solutions：The normal propyl alcohol peak area of sample solution；The ethanol of mixed standard solution in measure
With the ethanol peak area of the corresponding coefficient f2=mixed standard solution of normal propyl alcohol：The normal propyl alcohol peak area of mixed standard solution；It is mixed
In standardization solution, the content of ethanol is according to CEthanol=(f2 × V3 × V1 × 40)/(f1 × V2 × w) can be calculated, last
The ethanol content remained in calculating xanthan gum sample.
During step (5) are detected and recorded chromatogram using gas chromatograph, using for gas chromatograph is walked
It is rapid as follows：
A. open the carrier gas nitrogen of gas chromatograph；
B. open the air generator of gas chromatograph；
C., after air generator stable gas pressure, gas chromatograph host power supply is opened, and waits gas chromatograph self-inspection；
D. after self-inspection is finished, the computer that is connected with gas chromatograph is opened, opening N2000 works online station after start；
E. after gas chromatograph is ready, hydrogen generator is opened, 30 seconds right-hand man's moving points fire hydrogen after stable gas pressure
Flame detector；
F., after igniting is finished, zero point regulation is carried out within 10 minutes, and sample introduction starts detection after baseline is steady；
G., in detecting, after single injected sampling, when the record time of chromatogram reaches 10min, stop this sample introduction sample
Collection, prepares the next sample of detection.
Specific embodiment
It is below the present invention preferably embodiment, does not therefore define protection scope of the present invention.
The detection method of xanthan gum trace solvent residual quantity, is characterized in that the detection method step is as follows：
(1) prepare the standard solution of normal propyl alcohol：Concentration is prepared with chromatographically pure anhydrous normal propyl alcohol and redistilled water is
The normal propyl alcohol standard solution of 1mg/ml, it is standby；
(2) prepare the standard solution of ethanol：It is 1mg/ml that concentration is prepared with chromatographically pure dehydrated alcohol and redistilled water
Ethanol standard solution, it is standby；
(3) prepare mixed standard solution：Using the ethanol standard solution of the normal propyl alcohol standard solution and 1mg/ml of 1mg/ml
It is and redistilled water prepares mixed standard solution of the concentration for ethanol 0.04mg/ml and normal propyl alcohol 0.04mg/ml, standby；
(4) preparation of sample solution：First the xanthan gum sample by quality for w gram is placed in the round-bottomed flask of 500ml, then
The redistilled water for accurately measuring 200ml is added in this round-bottomed flask, then round-bottomed flask is fixed on agitator and is vibrated
1h, adds the defoamer of about 2ml, this round-bottomed flask is connected to distillation condensing units again then, is steamed after sample dissolving
Evaporate, distillation amount is V1 (about 100ml), and distillation amount V2 (about 95ml) for taking distillate is put in the volumetric flask of 100ml, finally
The normal propyl alcohol standard solution of 4ml is added, and finally 100ml (constant volume is V3=100ml) is settled to redistilled water, is sample
Product solution, it is standby；
(5) detected using gas chromatograph and record chromatogram：The temperature for controlling gas chromatographic column is 55 DEG C, injection port temperature
It is 200 DEG C to spend for 180 DEG C, checker temperature, and carrier gas during inspection is nitrogen；The mixed standard solution of 1ul is initially injected, is surveyed
Fixed, record chromatogram, determines peak height and peak width and calculates peak area；The sample solution of 1ul is then injected into, is measured, is recorded
Chromatogram, determines peak height and peak width and calculates peak area；
(6) calculate the ethanol content remained in xanthan gum sample：In measure, the ethanol and normal propyl alcohol of sample solution is corresponding
The ethanol peak area of coefficient f1=sample solutions：The normal propyl alcohol peak area of sample solution；The ethanol of mixed standard solution in measure
With the ethanol peak area of the corresponding coefficient f2=mixed standard solution of normal propyl alcohol：The normal propyl alcohol peak area of mixed standard solution；It is mixed
In standardization solution, the content of ethanol is according to CEthanol=(f2 × V3 × V1 × 40)/(f1 × V2 × w) can be calculated, last
The ethanol content remained in calculating xanthan gum sample.
During step (5) are detected and recorded chromatogram using gas chromatograph, using for gas chromatograph is walked
It is rapid as follows：
A. open the carrier gas nitrogen of gas chromatograph；
B. open the air generator of gas chromatograph；
C., after air generator stable gas pressure, gas chromatograph host power supply is opened, and waits gas chromatograph self-inspection；
D. after self-inspection is finished, the computer that is connected with gas chromatograph is opened, opening N2000 works online station after start；
E. after gas chromatograph is ready, hydrogen generator is opened, 30 seconds right-hand man's moving points fire hydrogen after stable gas pressure
Flame detector；
F., after igniting is finished, zero point regulation is carried out within 10 minutes, and sample introduction starts detection after baseline is steady；
G., in detecting, after single injected sampling, when the record time of chromatogram reaches 10min, stop this sample introduction sample
Collection, prepares the next sample of detection.
During being detected using gas chromatograph and recording chromatogram, it should also be noted that：During sample introduction, microsyringe should
Accomplish that turnover is quick, and be careful not to cause the bending of injector.
The inventive method has passed through substantial amounts of experiment and demonstration, and the conclusion for drawing is that the method is simple and easy to do, and accuracy is high,
Can verify that output is limited to the trace solvent content of 1ppm, be especially suitable for xanthan gum manufacturer and xanthan gum customer laboratory
Detection.
Claims (2)
1. the detection method of xanthan gum trace solvent residual quantity, is characterized in that the detection method step is as follows：
(1) prepare the standard solution of normal propyl alcohol：It is 1mg/ml that concentration is prepared with chromatographically pure anhydrous normal propyl alcohol and redistilled water
Normal propyl alcohol standard solution, it is standby；
(2) prepare the standard solution of ethanol：The second that concentration is 1mg/ml is prepared with chromatographically pure dehydrated alcohol and redistilled water
Alcohol standard solution, it is standby；
(3) prepare mixed standard solution：Using the ethanol standard solution and two of the normal propyl alcohol standard solution and 1mg/ml of 1mg/ml
Secondary distilled water prepares mixed standard solution of the concentration for ethanol 0.04mg/ml and normal propyl alcohol 0.04mg/ml, standby；
(4) preparation of sample solution：First the xanthan gum sample of quality w=4g is placed in the round-bottomed flask of 500ml, then accurately
The redistilled water for measuring 200ml is added in this round-bottomed flask, then round-bottomed flask is fixed on agitator and vibrates 1h, sample
The defoamer of about 2ml is added after product dissolving, this round-bottomed flask is connected to into distillation condensing units again then, is distilled, steam
The amount of evaporating V1 is 100ml, and distillation amount V2 for taking distillate is put in the volumetric flask of 100ml for 95ml, is eventually adding the normal propyl alcohol of 4ml
Standard solution, is finally settled to constant volume V3=100ml with redistilled water, is sample solution, standby；
(5) detected using gas chromatograph and record chromatogram：The temperature for controlling gas chromatographic column is 55 DEG C, injector temperature is
180 DEG C, checker temperature be 200 DEG C, during inspection carrier gas be nitrogen；The mixed standard solution of 1 μ l is initially injected, be measured,
Record chromatogram, determines peak height and peak width and calculates peak area；The sample solution of 1 μ l is then injected into, is measured, is recorded chromatograph
Figure, determines peak height and peak width and calculates peak area；
(6) calculate the ethanol content remained in xanthan gum sample：The corresponding coefficient of the ethanol and normal propyl alcohol of sample solution in measure
The ethanol peak area of f1=sample solutions：The normal propyl alcohol peak area of sample solution；The ethanol of mixed standard solution and just in measure
The ethanol peak area of the corresponding coefficient f2=mixed standard solution of propanol：The normal propyl alcohol peak area of mixed standard solution；Mixing mark
In quasi- solution, the content of ethanol is according to CEthanol=(f2 × V3 × V1 × 40)/(f1 × V2 × w) can be calculated, and can finally calculate
The ethanol content remained in xanthan gum sample.
2. the detection method of xanthan gum trace solvent residual quantity according to claim 1, is characterized in that the step (5) profit
During being detected and recorded chromatogram with gas chromatograph, the use step of gas chromatograph is as follows：
A. open the carrier gas nitrogen of gas chromatograph；
B. open the air generator of gas chromatograph；
C., after air generator stable gas pressure, gas chromatograph host power supply is opened, and waits gas chromatograph self-inspection；
D. after self-inspection is finished, the computer that is connected with gas chromatograph is opened, opening N2000 works online station after start；
E. after gas chromatograph is ready, hydrogen generator is opened, right-hand man's moving point combustion hydrogen flame inspection in 30 seconds after stable gas pressure
Survey device；
F., after igniting is finished, zero point regulation is carried out within 10 minutes, and sample introduction starts detection after baseline is steady；
G., in detecting, after single injected sampling, when the record time of chromatogram reaches 10min, stop the collection of this sample introduction sample,
Prepare the next sample of detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410507809.3A CN104391049B (en) | 2014-09-20 | 2014-09-20 | Detection method for residual quantity of xanthan gum microscale solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410507809.3A CN104391049B (en) | 2014-09-20 | 2014-09-20 | Detection method for residual quantity of xanthan gum microscale solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104391049A CN104391049A (en) | 2015-03-04 |
| CN104391049B true CN104391049B (en) | 2017-03-22 |
Family
ID=52608979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410507809.3A Active CN104391049B (en) | 2014-09-20 | 2014-09-20 | Detection method for residual quantity of xanthan gum microscale solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104391049B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108226354A (en) * | 2018-01-02 | 2018-06-29 | 上海信谊百路达药业有限公司 | A kind of detection method of budesonide residual solvent |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2791418C (en) * | 2010-03-10 | 2016-07-05 | Inovobiologic, Inc. | Food comprising glucomannan, xanthan gum and alginate for the treatment of metabolic disorders |
| CN102220393A (en) * | 2010-04-16 | 2011-10-19 | 淄博中轩生化有限公司 | Method for increasing dissolution rate of xanthan gum product |
-
2014
- 2014-09-20 CN CN201410507809.3A patent/CN104391049B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104391049A (en) | 2015-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Huang et al. | Protic ionic liquids for the selective absorption of H2S from CO2: thermodynamic analysis | |
| CN102798690B (en) | Method for detecting spirit by using chromatographic analysis of spirit | |
| Ji et al. | Phase equilibria of high pressure CO2 and deep eutectic solvents formed by quaternary ammonium salts and phenol | |
| CN105044234A (en) | Method for detecting specific migration amounts of thirteen methacrylic acids/esters in plastic product | |
| CN104007218A (en) | Determination method of bisphenol S transfer volume in plastic food packaging materials | |
| CN102680561A (en) | Method for measuring boric acid content in water-based adhesive for cigarettes | |
| CN104391049B (en) | Detection method for residual quantity of xanthan gum microscale solvent | |
| Badi et al. | Evaluation of reboiler temperature retention time on MEG degradation products at varying MEG concentrations | |
| CN111735884A (en) | High performance gas chromatography detection method for triethylamine content in feed liquid | |
| CN103149187A (en) | Fluorescent method for rapidly determining content of aliphatic acid | |
| CN202942115U (en) | Gas recovery rate determination device for detecting open type animal respiratory calorimetric system | |
| CN201611342U (en) | Automatic sample introduction Kjeldahl nitrogen determination apparatus | |
| CN203881388U (en) | Oil gas flowmeter | |
| CN108828123B (en) | Method for measuring content of butyraldehyde and paraldehyde in polyvinyl butyral resin | |
| CN101576499B (en) | Method and device for detecting concentration of dimethyl ether gas | |
| CN104569237A (en) | Method for determining methylal component in liquefied petroleum gas | |
| CN103267813A (en) | Method for detecting acrylonitrile migration volume in plastic product for acid food and application of method | |
| CN105974013A (en) | Gas chromatography detection method of content of essential oil | |
| CN105572279A (en) | Method for determining naphthalene content of coal tar through gas chromatography | |
| Song et al. | Isobaric vapor–liquid equilibrium for the binary systems of 1-butanol+ methoxy (methoxymethoxy) methane, and 1-butanol+ 2, 4, 6, 8-tetraoxanonane at 101.3 kPa | |
| CN105158374A (en) | VOC detecting device in hot-pressing process of wooden composite plate | |
| CN104390831A (en) | Method and device for preparing standard methacrylic acid gas sample | |
| CN212159079U (en) | Organic liquid fire extinguishing agent concentration test device that puts out a fire | |
| Guerra-Neto et al. | Bubble point determination for CO2+ ethanol+ alkanolamines (monoethanolamine, diethanolamine, or triethanolamine) at high pressures | |
| CN102156176A (en) | Method for measuring adipic acid content of air by gas chromatography |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| CB02 | Change of applicant information |
Address after: Dalate's 014300 city the Inner Mongolia Autonomous Region forest Erdos Zhao Zhen Shang Liang Industrial Park three Applicant after: Ordos Zhongxuan Biochemical Co., Ltd. Address before: Dalate's 014300 city the Inner Mongolia Autonomous Region forest Erdos Zhao Zhen Shang Liang Industrial Park three Applicant before: ORDOS ZHONGXUAN BIOCHEMICAL CO., LTD. |
|
| COR | Change of bibliographic data | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Jian Gang Tuo Inventor after: Dong Jinru Inventor before: Jian Gang Tuo Inventor before: Dong Jinru |