CN103728381A - Liquid chromatographic analysis method of aldehyde ketone compounds - Google Patents
Liquid chromatographic analysis method of aldehyde ketone compounds Download PDFInfo
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- CN103728381A CN103728381A CN201210389284.9A CN201210389284A CN103728381A CN 103728381 A CN103728381 A CN 103728381A CN 201210389284 A CN201210389284 A CN 201210389284A CN 103728381 A CN103728381 A CN 103728381A
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Abstract
The invention provides a liquid chromatographic analysis method of aldehyde ketone compounds. The conditions of liquid chromatography are: a chromatographic column of C18, 5um, 150*4.6mm (I.D.); a column temperature of 45 DEG C; a mobile phase comprising tetrahydrofuran, acetonitrile, and water; a detection wavelength of 360nm; and a sample size of 20ul. By optimization of the liquid chromatographic separation conditions, the method of the invention can effectively separate 15 aldehyde ketone compounds, meet the requirements for qualitative analysis, and has significant advantages of good separation degree, high precision, and low detecting limit.
Description
Technical field
The invention belongs to efficient liquid phase chromatographic analysis technical field, be specifically related to a kind of liquid phase chromatography analytical method of group compounds of aldehydes and ketones.
Background technology
Group compounds of aldehydes and ketones, as class air pollutants, has very large harm to human body, more and more causes people's attention.At present, formulate both at home and abroad and the environmental legislation of promulgating in all by multiple group compounds of aldehydes and ketones row people the hazardous contaminant list of priority control.In recent years, along with the development of the industries such as the raising of living standards of the people and chemical industry, the analysis to aldoketones organic contaminant in air and monitoring seem particularly important.In air, the assay method of group compounds of aldehydes and ketones mainly contains photometry, vapor-phase chromatography, high performance liquid chromatography etc.Although photometry is simple, the component measured is few, serious interference, sensitivity are low; And chromatography especially liquid phase chromatography owing to disturbing less, highly sensitive, good separating effect, be the ideal method of analyzing group compounds of aldehydes and ketones in air.But reality adopt liquid chromatography analysis formaldehyde, acetaldehyde, acryl aldehyde, acetone, propionic aldehyde, crotonaldehyde, butyraldehyde, benzaldehyde, isopentyl aldehyde, valeral, o-tolualdehyde ,/p-tolualdehyde, hexanal, 2, during 15 kinds of group compounds of aldehydes and ketones such as 5-dimethylbenzaldehyde, if it is improper that the conditioned disjunction mobile phase system of its liquid chromatography is selected, not effectively separation of propylene aldehyde-DNPH and two materials of acetone-DNPH, cannot effectively separate exactly several materials that retention time is the longest, exist that degree of separation is poor, the not high deficiency of precision.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, and a kind of liquid phase chromatography analytical method of group compounds of aldehydes and ketones is provided, and the method can make 15 kinds of group compounds of aldehydes and ketones effectively be separated, and degree of separation is good, and precision is high, and detection limit is low.
The present invention solves the problems of the technologies described above taked technical scheme: the liquid phase chromatography analytical method of group compounds of aldehydes and ketones, and the condition of described liquid chromatography is: chromatographic column: C18,5um, 150 × 4.6mm (I.D.); Column temperature: 45 ℃; Mobile phase composition comprises tetrahydrofuran, acetonitrile, water; Detect wavelength: 360nm; Sample size: 20ul.
As preferably, described method is taked gradient elution, and its gradient program is: when sample injection time is 0 minute, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 10 minutes, in mobile phase, the ratio of water is 65%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 10%; In the time of 15 minutes, in mobile phase, the ratio of water is 60%, and the ratio of acetonitrile is 40%, and the ratio of tetrahydrofuran is 0%; In the time of 60 minutes, in mobile phase, the ratio of water is 50%, and the ratio of acetonitrile is 50%, and the ratio of tetrahydrofuran is 0%; In the time of 70 minutes, in mobile phase, the ratio of water is 30%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 75 minutes, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 80 minutes, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%.
Compared with the existing technology, the present invention, by the optimization to liquid chromatography separation condition, can make 15 kinds of group compounds of aldehydes and ketones effectively be separated, and meets the requirement of qualitative analysis.In reversed-phase liquid chromatography, by changing the ratio of organic phase and water, the polarity of adjustable mobile phase, thus effectively improve mobile phase to the eluting power of adsorbed material and separation selectivity.Consider effectively separation of propylene aldehyde-DNPH and two materials of acetone-DNPH of acetonitrile-water system and methanol-water system, and tetrahydrofuran-acetonitrile-water system cannot effectively separate several materials that retention time is the longest.In order thoroughly to separate whole 15 kinds of Carbonyl compounds, therefore the present invention utilizes quaternary pump, two kinds of mobile phase systems have been adopted, first by tetrahydrofuran-acetonitrile-water system, separate the centralization compound occurring above, then by graded, mobile phase is progressively transitioned into acetonitrile-water system, thereby separates the compound occurring below.Result shows, has solved preferably a separation difficult problem for 15 kinds of Carbonyl compounds.Consider that sample size crosses conference and cause chromatographic column overload and pollute, the detectability of the other side's method that sample size crosses that I haven't seen you for ages, precision etc. impact simultaneously.So the present invention, according to conditions such as the granularity of the chromatographic column of selecting, post footpaths, is decided to be the most frequently used 20uL by sample size, taken into account preferably method accurately and equipment lives two aspect.Because the viscosity ratio of tetrahydrofuran-acetonitrile-water system is at room temperature larger, while causing HPLC to analyze, pressure is higher, so the present invention's column temperature is set to 45 ℃, reduces post and presses.Consider that it is 365nm that group compounds of aldehydes and ketones has 5 kinds of material maximum absorption wavelengths, separately have 6 kinds of material maximum absorption wavelength rates to be greater than 370nm, the maximum absorption wavelength of remaining material is in 360 left and right., under this wavelength, the absorbance of each component has all reached the more than 85% of its absorption maximum, has met the requirement of sensitivity for analysis.Therefore, the present invention selects 360nm as detecting wavelength.
Embodiment
Below in conjunction with embodiment, to of the present invention, be further elaborated.
Embodiment 1: a kind of liquid phase chromatography analytical method of group compounds of aldehydes and ketones, the condition of its high performance liquid chromatography is: chromatographic column: C18,5um, 150 × 4.6mm (I.D.); Column temperature: 45 ℃; Mobile phase composition comprises tetrahydrofuran, acetonitrile, water; Detect wavelength: 360nm; Sample size: 20ul; Described method is taked gradient elution, and its gradient program is: when sample injection time is 0 minute, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 10 minutes, in mobile phase, the ratio of water is 65%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 10%; In the time of 15 minutes, in mobile phase, the ratio of water is 60%, and the ratio of acetonitrile is 40%, and the ratio of tetrahydrofuran is 0%; In the time of 60 minutes, in mobile phase, the ratio of water is 50%, and the ratio of acetonitrile is 50%, and the ratio of tetrahydrofuran is 0%; In the time of 70 minutes, in mobile phase, the ratio of water is 30%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 75 minutes, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 80 minutes, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%.
Respectively 15 kinds of aldehyde ketone derivant standard solution are mixed with to 0.1,0.2,0.5,1.0,1.5,2.0,3.0, the solution of 4.0ug/mL, analyze, make standard colors spectrogram, again take peak area (y) as ordinate, aldehyde ketone content (ug/mL) be horizontal ordinate (x), drawing standard curve, calculate its regression equation by least square method, result shows that 15 kinds of Carbonyl compounds become good linear relationship, correlation coefficient r > 0.9995 in the concentration range of 0.1-4.0ug/mL.In blank sampling column, add the aldoketones derivant standard specimen of 5.0ug, then carry out pre-treatment and detection, result shows that average recovery rate is more than 97%; The mixed mark of aldehyde ketone of preparation low concentration (0.1/ml), replicate determination 5 times, with constant volume 2mL, sampling 5L calculates, and according to 3 times of snr computation minimum detectabilities, result detects and is limited to 2～16ug/m
3.
Though it is pointed out that above-described embodiment is to the present invention's detailed text description of contrasting, these text descriptions are the simple description to mentality of designing of the present invention just, rather than the restriction to thinking of the present invention.Any combination, increase or modification that is no more than mentality of designing of the present invention, all falls within the scope of protection of the present invention.
Claims (2)
1. the liquid phase chromatography analytical method of group compounds of aldehydes and ketones, is characterized in that, the condition of described liquid chromatography is: chromatographic column: C18,5um, 150 × 4.6mm (I.D.); Column temperature: 45 ℃; Mobile phase composition comprises tetrahydrofuran, acetonitrile, water; Detect wavelength: 360nm; Sample size: 20ul.
2. the liquid phase chromatography analytical method of group compounds of aldehydes and ketones according to claim 1, it is characterized in that taking gradient elution, its gradient program is: when sample injection time is 0 minute, in mobile phase, the ratio of water is 55%, the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 10 minutes, in mobile phase, the ratio of water is 65%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 10%; In the time of 15 minutes, in mobile phase, the ratio of water is 60%, and the ratio of acetonitrile is 40%, and the ratio of tetrahydrofuran is 0%; In the time of 60 minutes, in mobile phase, the ratio of water is 50%, and the ratio of acetonitrile is 50%, and the ratio of tetrahydrofuran is 0%; In the time of 70 minutes, in mobile phase, the ratio of water is 30%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 75 minutes, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%; In the time of 80 minutes, in mobile phase, the ratio of water is 55%, and the ratio of acetonitrile is 25%, and the ratio of tetrahydrofuran is 20%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104897814A (en) * | 2015-06-10 | 2015-09-09 | 广西大学 | Method for detecting aldehyde ketone concentration in atmosphere through combination of DNPH-silica-gel adsorption small columns and HPLC-UV |
| CN109596758A (en) * | 2018-11-24 | 2019-04-09 | 合肥谱尼测试科技有限公司 | Separate the liquid chromatogram mobile phase system of ten kinds of group compounds of aldehydes and ketones in plastic cement race track |
| CN114252533A (en) * | 2021-12-10 | 2022-03-29 | 一汽奔腾轿车有限公司 | Method for detecting aldehyde and ketone substance content in passenger car |
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| CN109596758A (en) * | 2018-11-24 | 2019-04-09 | 合肥谱尼测试科技有限公司 | Separate the liquid chromatogram mobile phase system of ten kinds of group compounds of aldehydes and ketones in plastic cement race track |
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Application publication date: 20140416 |