CN105675743A - Dimethylamine aqueous solution detection method - Google Patents
Dimethylamine aqueous solution detection method Download PDFInfo
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- CN105675743A CN105675743A CN201511035145.6A CN201511035145A CN105675743A CN 105675743 A CN105675743 A CN 105675743A CN 201511035145 A CN201511035145 A CN 201511035145A CN 105675743 A CN105675743 A CN 105675743A
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- dimethylamine
- dimethylamine agueous
- agueous solution
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- G—PHYSICS
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- 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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention relates to a dimethylamine aqueous solution detection method. The method comprises the following steps: 1, deriving a dimethylamine aqueous solution reference substance with 4-nitrobenzyl chloroformate; 2, detecting the derived dimethylamine aqueous solution reference substance through using a high performance liquid chromatograph with an ultraviolet detector; 3, drawing the standard curve of the dimethylamine aqueous solution; 4, deriving a sample to be detected; and 5, detecting dimethylamine in the sample to be detected according to a detection result obtained in step 2, and calculating the content of dimethylamine in the sample to be detected through using the standard curve. The dimethylamine aqueous solution detection method has the advantages of simple operation, sensitivity, fastness, low cost, and accurate and reliable result.
Description
Technical field
The present invention relates to a kind of technical field of analytical chemistry, especially a kind of dimethylamine agueous solution detection method.
Background technology
Dimethylamine be a kind of in the colourless inflammable gas of strong basicity, common is dimethylamine 40% aqueous solution, and the Monomethylamine of the existing production technique preparing dimethylamine agueous solution inevitably association trace, dimethylamine and Monomethylamine are low-grade aliphatic amine. Dimethylamine agueous solution is a kind of common Chemicals, is widely used in chemical production field. Mainly remove a mao agent, medicine (antibiotic), agricultural chemicals, textile industry solvent, dyestuff, explosive, propelling agent and dimethylhydrazine, N, the raw material of the organic intermediates such as dinethylformamide as vulcanization of rubber promotor, leather. Wherein dimethyl formamide is produced the dimethylamine consumed accounts for the 44.7% of total flow, and pesticide producing consumption accounts for 38.9%, medicine grade for production consumption and is accounted for 16.4%. At present in pharmaceutical industries, being widely used in the synthesis of the medicine such as meropenem, Walaphage, wherein the quality of amination reaction and product is had important impact by Monomethylamine content.
High performance liquid chromatography is analytical procedure conventional at present. High performance liquid chromatography with its separation efficiency height, highly sensitive, analysis speed is fast etc., and feature is widely used, the organic compound usable highly effective liquid-phase chromatographic analysis of more than 70 percent, particularly on the compartment analysis of high boiling point, macromole, strong polarity, poor heat stability compound, it is shown that advantage.
At present, the method for inspection of the dimethylamine reported has spectrophotometry, vapor-phase chromatography, gas chromatography-mass spectrography, ion chromatography, liquid phase chromatography, capillary electrophoresis and mass spectroscopy. Spectrophotometry generally adopts reagent Monomethylamine and dimethylamine to be derived, and generates the material with uv-absorbing, but the method sensitivity is low, efficiency is low and poor repeatability. Vapor-phase chromatography is the current detection topmost method of short-chain fat amine, but because of sample be the aqueous solution, capillary chromatographic column is easily produced damage by long-run analysis. According to HG/T2973, adopt packing to be checked by dimethylamine agueous solution, check consuming time longer, and low-grade aliphatic amine polarity is relatively big, easily causes tailing peak and poor repeatability. Gas chromatography mass spectrometry and mass spectroscopy complicated operation, consuming time longer. Ion chromatography analysis efficiency is higher, but some common positively charged ions can seriously affect detected result and expensive. Capillary electrophoresis is simple to operate, it is not necessary to derivative, but sensitivity is low, and the factor affecting electric osmose is more, and then have impact on repeatability. Liquid phase chromatography is the classical measurement method measuring low-grade aliphatic amine class content, owing to this compounds polarity is big, and the response value of liquid chromatogram detector is higher, acomia color group, unstressed configuration characteristic and characteristic ultraviolet absorption, thus often will first by its derivatize in case reach be easy to be separated, detection object. Column front derivation combines with high performance liquid chromatography and has that it is simple to operate, analysis time is short, and method is sensitive, linearity range width, and result accurately and reliably and the advantage such as popular wide, is therefore the strong instrument analyzing detection dimethylamine agueous solution.
Summary of the invention
The present invention is intended to solve the deficiencies in the prior art, and provides a kind of quick, repeatability height, dimethylamine agueous solution detection method with low cost simple to operate, sensitive.
The present invention for achieving the above object, by the following technical solutions: a kind of dimethylamine agueous solution detection method, it is characterised in that, comprise the following steps:
(1), nitrobenzyl chloroformate ester is used to be derived by dimethylamine agueous solution reference substance
Accurately take dimethylamine agueous solution reference substance respectively and it is placed in nessler colorimetric tube, shake 10min, stratification after adding water, nitrobenzyl chloroformate ester dichloromethane solution and methylene dichloride, take off a layer solution, 0.45 μm of filter membrane is crossed after diluting 500 times with methyl alcohol, for subsequent use;
(2), use high performance liquid chromatography to be equipped with UV-detector to be detected by derivative rear dimethylamine agueous solution reference substance;
(3), dimethylamine agueous solution typical curve is drawn
After dimethylamine agueous solution reference substance being detected with the instrument of step (2) and testing conditions, take sample weighting amount as ordinate zou, with peak area X-coordinate drawing standard curve;
(4), testing sample derivatize
Accurately take dimethylamine agueous solution sample and it is placed in nessler colorimetric tube, shake 10min, stratification after adding water, nitrobenzyl chloroformate ester dichloromethane solution and methylene dichloride, take off a layer solution, after diluting 500 times with methyl alcohol, cross 0.45 μm of filter membrane, for subsequent use;
(5) dimethylamine in testing sample is detected by detected result according to step (2), it may also be useful to typical curve calculates dimethylamine content in testing sample.
Preferably, the high performance liquid chromatography in described step (2) and step (5) is equipped with the testing conditions of UV-detector and is: Shimadzu LC-20AT high performance liquid chromatograph; Chromatographic column: C18250mm × 4.6mm, 5 μm; Flow velocity: 1.0mL/min; Determined wavelength: 254nm; Post temperature 40 DEG C; Sample size: 20 μ L; Moving phase: water-methanol; Working time: 25min.
Preferably, the gradient of described moving phase is:
The invention has the beneficial effects as follows: dimethylamine agueous solution detection method of the present invention, quick, with low cost, result simple to operate, sensitive is accurately and reliably.
Embodiment
The present invention is described in further detail by following examples, and following embodiment is explanation property, is not limited, can not limit protection scope of the present invention with following embodiment.
The method used in the present invention, if no special instructions, is ordinary method; The reagent used in the present invention or raw material, if no special instructions, be conventional commercially available prod.
Embodiment 1
A kind of dimethylamine agueous solution detection method, comprises the following steps:
(1), nitrobenzyl chloroformate ester is used to be derived by dimethylamine agueous solution reference substance
Accurately take dimethylamine agueous solution reference substance 0.1g, 0.3g, 0.5g, 0.75g, 1.0g respectively in 25mL nessler colorimetric tube, add 4.5mL water, 10min is shaken after 3mL nitrobenzyl chloroformate ester dichloromethane solution and 2mL methylene dichloride, stratification, take off a layer solution, 0.45 μm of filter membrane is crossed after diluting 500 times with methyl alcohol, for subsequent use;
(2), rear dimethylamine agueous solution reference substance detects to deriving to use high performance liquid chromatography to be equipped with UV-detector, and high performance liquid chromatography is equipped with the testing conditions of UV-detector and is: Shimadzu LC-20AT high performance liquid chromatograph; Chromatographic column: C18250mm × 4.6mm, 5 μm; Flow velocity: 1.0mL/min; Determined wavelength: 254nm; Post temperature 40 DEG C; Sample size: 20 μ L; Moving phase: water-methanol; Working time: 25min; Gradient is as follows:
(3), dimethylamine agueous solution typical curve is drawn
After dimethylamine agueous solution reference substance being detected with the instrument of step (2) and testing conditions, take sample weighting amount as ordinate zou, with peak area X-coordinate drawing standard curve;
(4), testing sample derivatize
Accurately take dimethylamine agueous solution sample 0.5g in 25mL nessler colorimetric tube, add 4.5mL water, after 3mL nitrobenzyl chloroformate ester dichloromethane solution and 2mL methylene dichloride, shake 10min, stratification, take off a layer solution, after diluting 500 times with methyl alcohol, cross 0.45 μm of filter membrane, for subsequent use;
(5) dimethylamine in testing sample is detected by detected result according to step (2), it may also be useful to typical curve calculates dimethylamine content in testing sample.
Embodiment 2
The repeatability of the dimethylamine of the inventive method is detected by the present embodiment, comprises the following steps:
Accurately take dimethylamine agueous solution reference substance 0.5g six parts respectively in 6 25mL nessler colorimetric tubes, add 4.5mL water, 10min is shaken after 3mL nitrobenzyl chloroformate ester dichloromethane solution and 2mL methylene dichloride, stratification, take off after layer solution methyl alcohol dilutes 500 times and cross 0.45 μm of filter membrane, for subsequent use, detection method with embodiment 1, according to the repeatability of the dimethylamine of Analysis result calculation the inventive method.
Embodiment 3
The recovery of standard addition of the dimethylamine of the inventive method is detected by the present embodiment, comprises the following steps:
Adopting the experiment of sample recovery of standard addition, add 500mg/mL dimethylamine agueous solution contrast solution 0.025mL, 0.05mL, 0.1mL respectively in the sample to which, correspondence adds scalar 12.5mg, 25mg, 50mg respectively, and deriving method is with embodiment 1; Each sample detection three times, detection method with embodiment 1, according to the recovery of standard addition of the dimethylamine of Analysis result calculation the inventive method.
Recovery of standard addition=(adding mark sample measured value-blank determination value) ÷ adds scalar × 100%.
Above to invention has been exemplary description; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the design of the method for the present invention and the various improvement that carry out of technical scheme, or directly apply to other occasion without improving, all within protection scope of the present invention.
Claims (3)
1. a dimethylamine agueous solution detection method, it is characterised in that, comprise the following steps:
(1), nitrobenzyl chloroformate ester is used to be derived by dimethylamine agueous solution reference substance
Accurately take dimethylamine agueous solution reference substance respectively and it is placed in nessler colorimetric tube, shake 10min, stratification after adding water, nitrobenzyl chloroformate ester dichloromethane solution and methylene dichloride, take off a layer solution, 0.45 μm of filter membrane is crossed after diluting 500 times with methyl alcohol, for subsequent use;
(2), use high performance liquid chromatography to be equipped with UV-detector to be detected by derivative rear dimethylamine agueous solution reference substance;
(3), dimethylamine agueous solution typical curve is drawn
After dimethylamine agueous solution reference substance being detected with the instrument of step (2) and testing conditions, take sample weighting amount as ordinate zou, with peak area X-coordinate drawing standard curve;
(4), testing sample derivatize
Accurately take dimethylamine agueous solution sample and it is placed in nessler colorimetric tube, shake 10min, stratification after adding water, nitrobenzyl chloroformate ester dichloromethane solution and methylene dichloride, take off a layer solution, after diluting 500 times with methyl alcohol, cross 0.45 μm of filter membrane, for subsequent use;
(5) dimethylamine in testing sample is detected by detected result according to step (2), it may also be useful to typical curve calculates dimethylamine content in testing sample.
2. dimethylamine agueous solution detection method according to claim 1, it is characterized in that, the high performance liquid chromatography in described step (2) and step (5) is equipped with the testing conditions of UV-detector and is: Shimadzu LC-20AT high performance liquid chromatograph;Chromatographic column: C18250mm × 4.6mm, 5 μm; Flow velocity: 1.0mL/min; Determined wavelength: 254nm; Post temperature 40 DEG C; Sample size: 20 μ L; Moving phase: water-methanol; Working time: 25min.
3. dimethylamine agueous solution detection method according to claim 2, it is characterised in that, the gradient of described moving phase is:
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109633046A (en) * | 2019-02-22 | 2019-04-16 | 成都倍特药业有限公司 | A method of detecting dimethylamine from duloxetine hydrochloride |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6100026A (en) * | 1995-04-25 | 2000-08-08 | Irori | Matrices with memories and uses thereof |
| CN1803758A (en) * | 2006-01-24 | 2006-07-19 | 浙江工业大学 | Method for synthesizing 4-nitrobenzyl chloroformate |
| CN101225069A (en) * | 2007-02-13 | 2008-07-23 | 天津市敬业精细化工有限公司 | Method for synthesizing meropenem intermediate |
| JP2008291207A (en) * | 2007-04-27 | 2008-12-04 | Kyowa Hakko Kirin Co Ltd | Helical polymer including basic amino acid |
| US20120244627A1 (en) * | 2009-10-26 | 2012-09-27 | Georgetown University | Methods for Quantifying Vitamin D Metabolites by Mass Spectrometry |
| CN103940936A (en) * | 2014-01-20 | 2014-07-23 | 天津市敬业精细化工有限公司 | Detection method of 4alpha-hydroxy-L-proline and trace L-proline in 4alpha-hydroxy-L-proline |
-
2015
- 2015-12-31 CN CN201511035145.6A patent/CN105675743B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6100026A (en) * | 1995-04-25 | 2000-08-08 | Irori | Matrices with memories and uses thereof |
| CN1803758A (en) * | 2006-01-24 | 2006-07-19 | 浙江工业大学 | Method for synthesizing 4-nitrobenzyl chloroformate |
| CN101225069A (en) * | 2007-02-13 | 2008-07-23 | 天津市敬业精细化工有限公司 | Method for synthesizing meropenem intermediate |
| JP2008291207A (en) * | 2007-04-27 | 2008-12-04 | Kyowa Hakko Kirin Co Ltd | Helical polymer including basic amino acid |
| US20120244627A1 (en) * | 2009-10-26 | 2012-09-27 | Georgetown University | Methods for Quantifying Vitamin D Metabolites by Mass Spectrometry |
| CN103940936A (en) * | 2014-01-20 | 2014-07-23 | 天津市敬业精细化工有限公司 | Detection method of 4alpha-hydroxy-L-proline and trace L-proline in 4alpha-hydroxy-L-proline |
Non-Patent Citations (4)
| Title |
|---|
| H. BRUCKNER ET AL: "Use of chromogenic and fluorescent oxycarbonyl chlorides as reagents for amino acid analysis by high-performance liquid chromatography", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| J. KIRSCHBAUM ET AL: "Determination of biogenic amines in fermented beverages and vinegars by pre-column derivatization withpara-nitrobenzyloxycarbonyl chloride (PNZ-Cl) and reversed-phase LC", 《CHROMATOGRAPHIA》 * |
| TOMOFUMI SANTA ET AL: "Derivatization reagents in liquid chromatography/electrospray ionization tandem mass spectrometry for biomedical analysis", 《DRUG DISCOV THER》 * |
| 罗海英 等: "高效液相色谱法测定工作场所空气中的二甲胺", 《中国卫生检验杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109633046A (en) * | 2019-02-22 | 2019-04-16 | 成都倍特药业有限公司 | A method of detecting dimethylamine from duloxetine hydrochloride |
| CN109633046B (en) * | 2019-02-22 | 2021-12-21 | 成都倍特药业股份有限公司 | Method for detecting dimethylamine from duloxetine hydrochloride |
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Application publication date: 20160615 Assignee: Gold Value (China) Financial Leasing Co.,Ltd. Assignor: TIANJIN JINGYE FINE CHEMICALS Co.,Ltd. Contract record no.: X2022980015639 Denomination of invention: A kind of dimethylamine aqueous solution detection method Granted publication date: 20190301 License type: Exclusive License Record date: 20220920 |