CN1963492A - Method for testing moisture content by sulfonyl isocyanate pre-column derivation method - Google Patents
Method for testing moisture content by sulfonyl isocyanate pre-column derivation method Download PDFInfo
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- CN1963492A CN1963492A CN 200610118933 CN200610118933A CN1963492A CN 1963492 A CN1963492 A CN 1963492A CN 200610118933 CN200610118933 CN 200610118933 CN 200610118933 A CN200610118933 A CN 200610118933A CN 1963492 A CN1963492 A CN 1963492A
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- sulfonyl isocyanate
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Abstract
This invention relates to sulfonylisocyanates resin column derived method to test water content in analysis chemical field, which comprises the following steps: using sulfonylisocyanates resin compound as derive agent added with hydroxyl group or sulfhydryl group compound to terminate reaction. The invention method is combined with high effective liquid phase spectrum and quantum spectrum, capillary electrophoresis or quantum spectrum or film spectrum method to realize the water accurate measurement.
Description
Technical field
The invention belongs to the analytical chemistry field, relate to the pre-column derivatization method of water, be specifically related to a kind of method that adopts the sulfonyl isocyanate pre-column derivatization method to measure moisture (being called for short the DZY method).
Background technology
The method of moisture mainly contains oven drying method, toluene method, hypobaric drying method, vapor-phase chromatography, expense Xiu Shi volumetric precipitation method, karl Fischer moisture titrator method etc. in the disclosed working sample of prior art.There is the shortcoming that operation is loaded down with trivial details, accuracy is low, be subject to disturb in methods such as above-mentioned oven drying method, toluene method, hypobaric drying method, expense Xiu Shi volumetric precipitation method; And the required instruments of method such as vapor-phase chromatography and karl Fischer moisture titrator method cost an arm and a leg and be difficult for to popularize.
In the research in analytical chemistry field, the researcher is seeking a kind of easily universal, cheap always, can method rapidly and efficiently, the high sensitivity measuring micro-moisture.
Summary of the invention
The object of the present invention is to provide a kind of pre-column derivatization method of water, the pre-column derivatization method of a kind of reaction conditions gentleness, water rapidly and efficiently especially is provided, be specifically related to adopt the sulfonyl isocyanate pre-column derivatization method to measure the method for moisture.
The inventive method is that derivatization reagent carries out pre-column derivatization with the sulfonyl isocyanate class, unite use with methods such as high performance liquid chromatography, high performance liquid chromatography-mass spectrum, Capillary Electrophoresis, capillary electrophoresis-mass spectrometry or thin-layered chromatography, can realize high sensitivity measuring micro-moisture in the sample.
The inventive method is achieved through the following technical solutions:
Get the sample that contains moisture to be measured, through after the sample pretreatment, add the reaction dissolvent that does not contain active hydrogen, and sulfonyl isocyanate class derivatization reagent, mixing was placed 1-20 minute under the room temperature, added hydroxyl or sulfhydryl compound cessation reaction, methods such as connection and use high performance liquid chromatography, high performance liquid chromatography-mass spectrum, Capillary Electrophoresis, capillary electrophoresis-mass spectrometry or thin-layered chromatography, the concentration of mensuration moisture.Undertaken by following step:
1) pre-service aqueous specimen to be measured according to a conventional method,
2) add reaction dissolvent and the sulfonyl isocyanate class derivatization reagent that does not contain active hydrogen, mixing,
3) room temperature was placed 1-20 minute, added hydroxyl or sulfhydryl compound cessation reaction,
4) content of usefulness high performance liquid chromatography, high performance liquid chromatography-mass spectrum, Capillary Electrophoresis, capillary electrophoresis-mass spectrometry method or tlc determination moisture.
The described derivatization reagent of the inventive method is the sulfonyl isocyanate compounds, and its general structure can be expressed as RSO
2NCO, wherein R can be the alkyl or aryl group.
The present invention uses the sulfonyl isocyanate compounds as derivatization reagent, and derivative reaction at room temperature promptly can take place.After described derivatization reagent and solution mixing to be measured only needed 1-20 minute, derivative reaction was promptly finished.
The described solvent that does not contain active hydrogen of the inventive method be acetonitrile, tetrahydrochysene bark mutter, ether, benzene, toluene or phenixin equal solvent.
The inventive method can be passed through multiple instrument such as high performance liquid chromatography, high performance liquid chromatography-mass spectrum, Capillary Electrophoresis, capillary electrophoresis-mass spectrometry or thin-layer chromatography and realize, particularly high performance liquid chromatography-UV-detector has advantages such as universal, cheapness.The inventive method compared with the prior art, have measure quick, accurate, easy, be easy to promote, cost is low, reaction conditions is gentle, side reaction product is few and excessive derivatization reagent can not disturb the advantages such as mensuration of determinand.
Description of drawings
Fig. 1 is blank acetonitrile derivatization high performance liquid chromatography (HPLC) figure,
Wherein, interior mark chromatographic peak, water derivatization product chromatographic peak, methyl alcohol derivatization product chromatographic peak baseline separation; Acetonitrile contains micro-moisture and therefore still has water derivatization product chromatographic peak.
Fig. 2 contains water-acetonitrile derivatization high performance liquid chromatography (HPLC) figure, interior mark chromatographic peak, water derivatization product chromatographic peak, methyl alcohol derivatization product chromatographic peak baseline separation among the figure.
Fig. 3 is enteral nutrition powder sample acetonitrile solution derivatization high performance liquid chromatography (HPLC) figure, and interior mark chromatographic peak, water derivatization product chromatographic peak, methyl alcohol derivatization product chromatographic peak baseline separation are not seen impurity chromatographic peak interference test among the figure,
Wherein, the 1st, interior mark (p-aminobenzoic acid);
The 2nd, water derivatization product;
The 3rd, methyl alcohol derivatization product.
Embodiment
Embodiment 1
Instrument and condition:
Day island proper Tianjin 10A type highly effective liquid phase chromatographic system comprises binary gradient system, column temperature control box, UV, visible light variable-wavelenght detector, Hangzhou English spectrum HS2000 workstation and 20 μ L hand sampling systems; Chromatographic column: 150 * 4.6mm ID, 5 μ m Diamonsil
TMC
18(DIKMA); Water: take by weighing 0.69gKH
2PO
4Being dissolved in the 500ml pure water, is 2.5 with the phosphorus acid for adjusting pH value again.Organic phase: acetonitrile.The geometric ratio wash-out, water: organic phase=55: 45; Flow velocity: 1.0mL/min; Column temperature: 25 ℃; Detect wavelength: 227nm; Sample size: 20 μ L.
Experimental procedure:
Precision takes by weighing water 200mg, places the 10mL volumetric flask, and acetonitrile dissolving also is diluted to scale, is mixed with the reference substance storing solution of concentration 20mg/mL, again with dilution in acetonitrile to 20mg/mL, 10mg/mL, 5mg/mL, 3mg/mL, the concentration of 2mg/mL is for the preparation standard curve.
Get 50 μ L titers, add 20% tolysulfonyl isocyanates (v/v) acetonitrile solution, 100 μ L, the whirlpool mixing, room temperature was placed 20 minutes, treat that it fully reacts after, add 50 μ L methyl alcohol and remove unreacted derivatization reagent.Get 50 μ L reactant liquors and add 23mg/ml p-aminobenzoic acid acetonitrile inner mark solution 100 μ L, add the 2mL acetonitrile solution again, the whirlpool mixing.With 1000 times of dilution in acetonitrile, sample introduction 20 μ L, blank with doing retinue.Mark and water derivatization product peak area in the record are with both ratio calculation linear equations.
Precision takes by weighing enteral nutrition powder 6.28g, place the 50mL volumetric flask, the acetonitrile dissolving also is diluted to scale, getting 50 μ L and titer equally prepares with the same terms, identical chromatographic conditions sample introduction 20 μ L, mark and water derivatization product peak area in the record are in both ratio substitution linear equations, calculate its measured value, calculated value is calculated moisture divided by actual sampling amount.
Claims (5)
1, the sulfonyl isocyanate pre-column derivatization method is measured the method for moisture, after it is characterized in that the testing sample pre-service, add the reaction dissolvent that does not contain active hydrogen, with the sulfonyl isocyanate class is that derivatization reagent carries out pre-column derivatization, with high performance liquid chromatography, high performance liquid chromatography-mass spectrum, Capillary Electrophoresis, capillary electrophoresis-mass spectrometry or thin-layered chromatography connection and use, measure moisture.
2, sulfonyl isocyanate pre-column derivatization method according to claim 1 is measured the method for moisture, it is characterized in that described derivatization reagent is the sulfonyl isocyanate compounds, and its general structure is RSO
2NCO, wherein R is the alkyl or aryl group.
3, the sulfonyl isocyanate pre-column derivatization method of water according to claim 1 is measured the method for moisture, it is characterized in that being undertaken by following step:
1) aqueous specimen pre-service to be measured,
2) add reaction dissolvent and the sulfonyl isocyanate class derivatization reagent that does not contain active hydrogen, mixing,
3) room temperature was placed 1-20 minute, added hydroxyl or sulfhydryl compound cessation reaction,
4) with moisture in high performance liquid chromatography, high performance liquid chromatography-mass spectrum, Capillary Electrophoresis, capillary electrophoresis-mass spectrometry method or the tlc determination sample.
4, method according to claim 3 is characterized in that the described reaction dissolvent that does not contain active hydrogen is selected from acetonitrile, tetrahydrofuran, ether, benzene, toluene or phenixin.
5, method according to claim 3 is characterized in that described derivative reaction is that room temperature was placed 1-20 minute, and reaction finishes, and adds hydroxyl or sulfhydryl compound cessation reaction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610118933 CN1963492A (en) | 2006-11-29 | 2006-11-29 | Method for testing moisture content by sulfonyl isocyanate pre-column derivation method |
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| CN 200610118933 CN1963492A (en) | 2006-11-29 | 2006-11-29 | Method for testing moisture content by sulfonyl isocyanate pre-column derivation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597185A (en) * | 2014-12-25 | 2015-05-06 | 四川大学 | Detection method for simultaneously measuring three kinds of isocyanates by using precolumn derivatization-gas chromatography-mass spectrography |
| CN113583062A (en) * | 2021-07-26 | 2021-11-02 | 华南农业大学 | Derivatization method of lincomycin, lincomycin derivative and application of derivatization method |
| CN114112965A (en) * | 2020-08-31 | 2022-03-01 | 万华化学集团股份有限公司 | Method for detecting trace moisture in isocyanate and application of method in online monitoring |
| CN114527220A (en) * | 2022-03-04 | 2022-05-24 | 杭州师范大学 | Method for quantifying trace silicon hydroxyl in organic silicon raw rubber |
-
2006
- 2006-11-29 CN CN 200610118933 patent/CN1963492A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104597185A (en) * | 2014-12-25 | 2015-05-06 | 四川大学 | Detection method for simultaneously measuring three kinds of isocyanates by using precolumn derivatization-gas chromatography-mass spectrography |
| CN114112965A (en) * | 2020-08-31 | 2022-03-01 | 万华化学集团股份有限公司 | Method for detecting trace moisture in isocyanate and application of method in online monitoring |
| CN114112965B (en) * | 2020-08-31 | 2024-04-09 | 万华化学集团股份有限公司 | Method for detecting trace moisture in isocyanate and application of method in online monitoring |
| CN113583062A (en) * | 2021-07-26 | 2021-11-02 | 华南农业大学 | Derivatization method of lincomycin, lincomycin derivative and application of derivatization method |
| CN114527220A (en) * | 2022-03-04 | 2022-05-24 | 杭州师范大学 | Method for quantifying trace silicon hydroxyl in organic silicon raw rubber |
| CN114527220B (en) * | 2022-03-04 | 2023-11-17 | 杭州师范大学 | Quantitative method for trace silicon hydroxyl in organosilicon raw rubber |
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