CN106226410A - Measure the method for carbamide in water body - Google Patents
Measure the method for carbamide in water body Download PDFInfo
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- CN106226410A CN106226410A CN201610513071.0A CN201610513071A CN106226410A CN 106226410 A CN106226410 A CN 106226410A CN 201610513071 A CN201610513071 A CN 201610513071A CN 106226410 A CN106226410 A CN 106226410A
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- water
- carbamide
- water body
- mensuration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention discloses the method for urea content in water body that measures, it is characterised in that include step: A), water sampling；B), high performance liquid chromatograph analysis water-like is used；Wherein, flowing is acetonitrile and water mutually, and volume ratio is (90 98): (10 2)；Atomization drying temperature is 15 DEG C 30 DEG C.In mensuration water body in the present invention, the method for carbamide, uses better simply liquid-liquid extraction, can reduce the interference of water body mesostroma.In separation process, use HILIC 1 mixed-matrix chromatographic column, the stick effect of carbamide can be improved.Meanwhile, use highly sensitive CAD detector, the problem that ultraviolet end absorption interferes when detecting can be avoided, it is easy to accurate quantitative analysis.In general, the method is the most simple to operate, be prone to grasp, can be as the mensuration of the carbamide in the substrate such as water body.The method using the present invention, in water body, the detection limit of carbamide can reach nanogram level.
Description
Technical field
The present invention relates to measure the method for carbamide in water body.
Background technology
Carbamide (Urea) is also known as urea or phosphoamide, and molecular formula is H2NCONH2, CAS accession number: 57-13-6, it is a kind of white
Color crystal, soluble in water, belong to highly polar ultraviolet end absorption compound.Having many uses of carbamide, uses more, a lot
Being required in application detecting its content, therefore detection method is the most varied.Such as, Wang Jianfei etc. use the inspection of liquid chromatograph ultraviolet
Survey device method, with pure water for flowing phase, use ODS chromatographic column to separate, ultraviolet detection wavelength 190nm, determine the carbamide in soil
Content, detection limit reach 0.3mg/L；The research such as Wang Yubo uses HILIC modal cutoff, and UV-detector method determines breast system
Carbamide in product, have employed polar-silica chromatographic column, and flowing is phosphate mutually: acetonitrile (20:80), ultraviolet wavelength 200nm
Detecting, the method preferably can separate with compounds such as tripolycyanamide, disturbs less, can carry out the most quantitative.
Wang Zuxiang etc. use high performance liquid chromatography-tandem mass method to measure carbamide, biuret and the dicyandiamide in food, use Zic-
HILIC post separates, and electron spray positive ion electrospray is from (ESI+) pattern and many reaction monitorings (MRM) scan pattern, and external standard is legal
Amount, result shows that the detection of carbamide is limited to 0.03mg/L.Other detection application processes also have bright grade of Dong Chun to use reversed phase high performance liquid
Phase chromatography measures the carbamide in animal feed；Wang Xiaojuan etc.[5]Nh 2 column is used to determine the urea content in yellow wine；
Kodama etc. detect the carbamide in wine to OPA as column front derivation agent, employing fluorescence detection, improve carbamide detection
Sensitivity, reach detection and be limited to 0.003mg/L, etc..But, in above detection method, the retention time of carbamide is short.With
Time, owing to carbamide uv absorption is poor, need to use the wavelength of about 190nm, which results in increase and detection that background absorbs
The unstability of device.And, its testing result lower limit is higher, it is impossible to meet the testing requirement day by day improved.
Summary of the invention
An object of the present invention is to overcome deficiency of the prior art, it is provided that the mensuration water that a kind of detection limit is lower
The method of carbamide in body.
For realizing object above, it is achieved through the following technical solutions:
Measure the method for urea content in water body, it is characterised in that include step:
A), water sampling；
B), high performance liquid chromatograph analysis water-like is used；Wherein, flowing is acetonitrile and water mutually, and volume ratio is (90-98):
(10-2)；Atomization drying temperature is 15 DEG C-30 DEG C.
According to one embodiment of present invention, the chromatographic column in described efficient liquid phase chromatographic analysis instrument is HILIC-1.
According to one embodiment of present invention, described acetonitrile is (95-98) with the volume ratio of water: (5-2).
According to one embodiment of present invention, described atomization drying temperature is 18 DEG C-22 DEG C.
According to one embodiment of present invention, data acquiring frequency is 1-10Hz.
In mensuration water body in the present invention, the method for carbamide, uses better simply liquid-liquid extraction, can reduce water body mesostroma
Interference.In separation process, use HILIC-1 mixed-matrix chromatographic column, the stick effect of carbamide can be improved.Meanwhile, as joined
Close highly sensitive CAD detector, the problem that ultraviolet end absorption interferes when detecting can be avoided, it is easy to accurate quantitative analysis divides
Analysis.In general, the method is the most simple to operate, be prone to grasp, can be as the mensuration of the carbamide in the substrate such as water body.Use
The method of the present invention, in water body, the detection limit of carbamide can reach nanogram level.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail:
Measure the method for urea content in water body, including step:
A), water sampling；
B), using the chromatographic column in efficient liquid phase chromatographic analysis instrument described in high performance liquid chromatograph analysis water-like is HILIC-
1.；Wherein, flowing is acetonitrile and water mutually, and volume ratio is (90-98): (10-2), is preferably (95-98): (5-2).Atomization drying
Temperature is 15 DEG C-30 DEG C, preferably 18 DEG C-22 DEG C.Data acquiring frequency is 1-10Hz.
Embodiment 1
A), water sampling；
B), using the chromatographic column in efficient liquid phase chromatographic analysis instrument described in high performance liquid chromatograph analysis water-like is HILIC-
1.Wherein, flowing is acetonitrile and water mutually, and volume ratio is 90:10.Atomization drying temperature is 15 DEG C.Data acquiring frequency is 5Hz.
Embodiment 2
A), water sampling；
B), using the chromatographic column in efficient liquid phase chromatographic analysis instrument described in high performance liquid chromatograph analysis water-like is HILIC-
1.Wherein, flowing is acetonitrile and water mutually, and volume ratio is 95:5.Atomization drying temperature is 25 DEG C.Data acquiring frequency is 2Hz.
Embodiment 3
A), water sampling；
B), using the chromatographic column in efficient liquid phase chromatographic analysis instrument described in high performance liquid chromatograph analysis water-like is HILIC-
1.Wherein, flowing is acetonitrile and water mutually, and volume ratio is 97:3.Atomization drying temperature is 20 DEG C.Data acquiring frequency is 5Hz.
Embodiment 4
A), water sampling；
B), using the chromatographic column in efficient liquid phase chromatographic analysis instrument described in high performance liquid chromatograph analysis water-like is HILIC-
1.Wherein, flowing is acetonitrile and water mutually, and volume ratio is 98:10.Atomization drying temperature is 30 DEG C.Data acquiring frequency is 10Hz.
Operating procedure condition according to embodiment 3
Preparation 5,10,20 μ g/ml carbamide standard working solution, are measured by embodiment 3 chromatographic condition, and calculating the response rate is
98.0%～101.0%.Testing result is as shown in table 1.
Table 1 sample recovery testu
Through experiment, the scheme in the present invention and each embodiment, all can reach the effect suitable with embodiment 3, error rate is equal
Less than 2%.
In mensuration water body in the present invention, the method for carbamide, uses better simply liquid-liquid extraction, can reduce water body mesostroma
Interference.In separation process, use HILIC-1 mixed-matrix chromatographic column, the stick effect of carbamide can be improved.Meanwhile, as joined
Close highly sensitive CAD detector, the problem that ultraviolet end absorption interferes when detecting can be avoided, it is easy to accurate quantitative analysis divides
Analysis.In general, the method is the most simple to operate, be prone to grasp, can be as the mensuration of the carbamide in the substrate such as water body.Use
The method of the present invention, in water body, the detection limit of carbamide can reach nanogram level.
Embodiment in the present invention is only used for that the present invention will be described, is not intended that the restriction to right,
Those skilled in that art it is contemplated that other replacements being substantially equal to, the most within the scope of the present invention.
Claims (5)
1. measure the method for urea content in water body, it is characterised in that include step:
A), water sampling；
B), high performance liquid chromatograph analysis water-like is used；Wherein, flowing is acetonitrile and water mutually, and volume ratio is (90-98): (10-
2)；Atomization drying temperature is 15 DEG C-30 DEG C.
The method of urea content in mensuration water body the most according to claim 1, it is characterised in that described high performance liquid chromatography
Chromatographic column in analyser is HILIC-1.
The method of urea content in mensuration water body the most according to claim 1, it is characterised in that described acetonitrile and the body of water
Long-pending ratio is (95-98): (5-2).
The method of urea content in mensuration water body the most according to claim 1, it is characterised in that described atomization drying temperature
It it is 18 DEG C-22 DEG C.
The method of urea content in mensuration water body the most according to claim 1, it is characterised in that data acquiring frequency is 1-
10Hz。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610513071.0A CN106226410A (en) | 2016-07-01 | 2016-07-01 | Measure the method for carbamide in water body |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610513071.0A CN106226410A (en) | 2016-07-01 | 2016-07-01 | Measure the method for carbamide in water body |
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| CN201610513071.0A Pending CN106226410A (en) | 2016-07-01 | 2016-07-01 | Measure the method for carbamide in water body |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107247103A (en) * | 2017-07-31 | 2017-10-13 | 黄河三角洲京博化工研究院有限公司 | A kind of method of thiocarbamide content in utilization HPLC external standard methods thiocarbamide synthesis |
| CN110187031A (en) * | 2019-06-12 | 2019-08-30 | 贵州联盛药业有限公司 | The measuring method of urea content in a kind of Moschus blood-circulation and removing blood stasis ointment |
| CN110954640A (en) * | 2020-01-02 | 2020-04-03 | 四川金象赛瑞化工股份有限公司 | Method for detecting trace urea in melamine |
| CN113514588A (en) * | 2021-06-02 | 2021-10-19 | 原子高科股份有限公司 | High performance liquid chromatography analysis method of relevant substances of cysteamine for injection |
| CN115326948A (en) * | 2022-07-05 | 2022-11-11 | 南通群安电子材料有限公司 | Method for measuring content of various organic bases in membrane removing liquid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003102220A2 (en) * | 2002-06-04 | 2003-12-11 | The Institute For Systems Biology | Methods for high throughput and quantitative proteome analysis |
| CN102928530A (en) * | 2012-10-15 | 2013-02-13 | 谱尼测试科技股份有限公司 | Detection method for measuring residual quantity of urea in bean sprout by high performance liquid chromatography |
| CN104101664A (en) * | 2014-07-31 | 2014-10-15 | 国家烟草质量监督检验中心 | Method for measuring urea content of paper |
| CN104142373A (en) * | 2014-07-31 | 2014-11-12 | 国家烟草质量监督检验中心 | Method for determining urea content in additives |
-
2016
- 2016-07-01 CN CN201610513071.0A patent/CN106226410A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003102220A2 (en) * | 2002-06-04 | 2003-12-11 | The Institute For Systems Biology | Methods for high throughput and quantitative proteome analysis |
| CN102928530A (en) * | 2012-10-15 | 2013-02-13 | 谱尼测试科技股份有限公司 | Detection method for measuring residual quantity of urea in bean sprout by high performance liquid chromatography |
| CN104101664A (en) * | 2014-07-31 | 2014-10-15 | 国家烟草质量监督检验中心 | Method for measuring urea content of paper |
| CN104142373A (en) * | 2014-07-31 | 2014-11-12 | 国家烟草质量监督检验中心 | Method for determining urea content in additives |
Non-Patent Citations (3)
| Title |
|---|
| THOMAS A.WALKER 等: "A liquid chromatographic assay for urea in over-the-counter carbamide peroxide products", 《JOURNAL OF PHARMACEUTICAL&BIOMEDICAL ANALYSIS》 * |
| 张大为 等: "一种新型的采用 HILIC色谱柱与电雾式检测器测定水体中尿素的方法", 《广东化工》 * |
| 杜光宇 等: "高效液相色谱法测定游泳池水中尿素含量", 《中国卫生工程学》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107247103A (en) * | 2017-07-31 | 2017-10-13 | 黄河三角洲京博化工研究院有限公司 | A kind of method of thiocarbamide content in utilization HPLC external standard methods thiocarbamide synthesis |
| CN107247103B (en) * | 2017-07-31 | 2019-10-11 | 黄河三角洲京博化工研究院有限公司 | A method of utilizing thiocarbamide content in the synthesis of HPLC external standard method thiocarbamide |
| CN110187031A (en) * | 2019-06-12 | 2019-08-30 | 贵州联盛药业有限公司 | The measuring method of urea content in a kind of Moschus blood-circulation and removing blood stasis ointment |
| CN110954640A (en) * | 2020-01-02 | 2020-04-03 | 四川金象赛瑞化工股份有限公司 | Method for detecting trace urea in melamine |
| CN110954640B (en) * | 2020-01-02 | 2022-08-23 | 四川金象赛瑞化工股份有限公司 | Method for detecting trace urea in melamine |
| CN113514588A (en) * | 2021-06-02 | 2021-10-19 | 原子高科股份有限公司 | High performance liquid chromatography analysis method of relevant substances of cysteamine for injection |
| CN115326948A (en) * | 2022-07-05 | 2022-11-11 | 南通群安电子材料有限公司 | Method for measuring content of various organic bases in membrane removing liquid |
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Application publication date: 20161214 |