CN103675110B - The separation of a kind of tetrabromobisphenol A composition and analysis determining method - Google Patents
The separation of a kind of tetrabromobisphenol A composition and analysis determining method Download PDFInfo
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- CN103675110B CN103675110B CN201210322026.9A CN201210322026A CN103675110B CN 103675110 B CN103675110 B CN 103675110B CN 201210322026 A CN201210322026 A CN 201210322026A CN 103675110 B CN103675110 B CN 103675110B
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Abstract
The invention discloses that the object of the present invention is achieved like this: the separation of a kind of tetrabromobisphenol A composition and analysis determining method, it uses high performance liquid chromatograph, it is the chromatographic column of filler with octadecyl silane, with mixtures of eluents for flowing phase, use the method for gradient elution that the composition in tetrabromobisphenol A sample solution is detected.Method for separating and analyzing of the present invention, available chromatograph carries out quantitative analysis to each composition of tetrabromobisphenol A, reaches the purpose of quality management and control.
Description
Technical field
Having the present invention relates to chemical composition analysis method, particularly one utilizes high performance liquid chromatography to enter tetrabromobisphenol A
Row composition separates the method analyzed.
Background technology
Tetrabromobisphenol A is one of conventional brominated flame retardant, the primary raw material of brominated epoxy resin.Chemistry is entitled: 2,
2 ', 6,6 '-TETRABROMOBISPHENOL A structural formulas are:
Molecular formula is C15H12Br4O, molecular weight: 544
The composition beyond tetrabromobisphenol A that manufacture process produces also has:
MONOBROMOBISPHENOL A:
Molecular formula is C15H15BrO2, molecular weight: 307
DIBROMOBISPHENOL A:
Molecular formula is C15H14Br2O2, molecular weight: 386
TRIBROMOBISPHENOL A:
Molecular formula is C15H13Br3O2, molecular weight: 465
At present, do not have in the industry tetrabromobisphenol A purity, the assay method fast and accurately of impurity content.
Summary of the invention
It is an object of the invention to provide separation and the analysis determining method of a kind of tetrabromobisphenol A composition, can effectively, soon
Speed, accurately the tetrabromobisphenol A after dissociating is carried out component analysis, it is achieved thereby that the control of each composition of tetrabromobisphenol A, quality
Controlling party face has important practical significance.
The object of the present invention is achieved like this: the separation of a kind of tetrabromobisphenol A composition and analysis determining method, its feature
It is: use high performance liquid chromatograph, be the chromatographic column of filler with octadecyl silane, with mixtures of eluents for flowing
Phase, uses the method for gradient elution to detect the composition in tetrabromobisphenol A sample solution.
Described chromatographic column uses specification to be 250mm × 4.6mm, the chromatographic column of 5 μm.
During described detection, the column temperature of chromatographic column is 30 DEG C.
Described mixtures of eluents is the mixture of acetonitrile and water.
In described acetonitrile and the mixture of water, both volume ratios are acetonitrile: water=50:50～0:100.
The described method using gradient elution is in 0～30min, acetonitrile: the volume ratio of water is from 50:50 even variation
To 0:100.
Described flow rate of mobile phase is 0.8ml/min.
The concentration of described tetrabromobisphenol A sample solution is 0.01g/ml acetonitrile, and sampling volume is 20 μ l.
Wavelength during described detection is 254nm.
Described high performance liquid chromatograph is Agilent 1100.
Method for separating and analyzing of the present invention, available chromatograph carries out quantitative analysis to each composition of tetrabromobisphenol A, reaches
Purpose to quality management and control.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1, the high performance liquid chromatography composition separation analysis chart of tetrabromobisphenol A sample A.
Fig. 2 is the embodiment of the present invention 2, the high performance liquid chromatography composition separation analysis chart of tetrabromobisphenol A sample B.
Detailed description of the invention
The present invention is separation and the analysis determining method of a kind of tetrabromobisphenol A composition, and it uses high performance liquid chromatograph, uses
Octadecyl silane is the chromatographic column of filler, with mixtures of eluents for flowing phase, uses the method for gradient elution to four
Composition in bromine bisphenol-A sample solution detects.
Preferably, chromatographic column uses specification to be 250mm × 4.6mm, the chromatographic column of 5 μm.During detection, the column temperature of chromatographic column is
30℃.Preferably, mixtures of eluents is the mixture of acetonitrile and water.In the mixture of acetonitrile and water, both volume ratios are acetonitrile
: water=50:50～0:100.The method using gradient elution is in 0～30min, acetonitrile: the volume ratio of water is uniform from 50:50
It is changed to 0:100.Preferably, flow rate of mobile phase is 0.8ml/min.Preferably, the concentration of tetrabromobisphenol A sample solution is
0.01g/ml acetonitrile, sampling volume is 20 μ l.Wavelength during detection is 254nm.High performance liquid chromatograph is Agilent 1100.
Qualitative analysis is carried out for tetrabromobisphenol A composition, only need to use mass spectrograph (LC-MS) when analyzing first, utilize
Its ion mass-to-charge ratio is different, separates the molecule of different molecular weight, measures molecular weight and carries out composition and structural analysis, by analysis
I.e. can confirm existing each go out peak corresponding be the material of which kind of structure.
Below by specific example, invention is described in further details, but the present invention is not limited to this specific examples.
Embodiment 1
Instrument and condition
High performance liquid chromatograph: Agilent 1100
Chromatographic column: octadecyl silane is the chromatographic column (250mm × 4.6mm, 5 μm) of filler
Flowing phase: acetonitrile: water=50:50～0:100(volume ratio)
Condition of gradient elution: 0～30min, acetonitrile: the ratio of water is from 50:50(volume ratio) even variation is to 0:100(body
Long-pending ratio).
Detection wavelength: 254nm
Column temperature: 30 DEG C
Sampling volume: 20 μ l
Experimental procedure: weigh tetrabromobisphenol A sample A 0.1g, be placed in 10ml volumetric flask, adds acetonitrile and dissolves, and be diluted to
Scale, shakes up, and as test sample solution, carries out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, records chromatogram, knot
Fruit sees Fig. 1.
Each composition result:
| Retention time (min) | Composition | Content (%) |
| 5.058 | MONOBROMOBISPHENOL A | 0.54 |
| 11.466 | TRIBROMOBISPHENOL A | 0.91 |
| 14.329 | TETRABROMOBISPHENOL A | 98.04 |
| 22.423～23.383 | Other | 0.51 |
Embodiment 2
Instrument and condition
High performance liquid chromatograph: Agilent 1100
Chromatographic column: octadecyl silane is the chromatographic column (250mm × 4.6mm, 5 μm) of filler
Flowing phase: acetonitrile: water=50:50～0:100(volume ratio)
Condition of gradient elution: 0～30min, acetonitrile: the ratio of water is from 50:50(volume ratio) even variation is to 0:100(body
Long-pending ratio).
Detection wavelength: 254nm
Column temperature: 30 DEG C
Sampling volume: 20 μ l
Experimental procedure: weigh tetrabromobisphenol A sample B 0.1g, be placed in 10ml volumetric flask, adds acetonitrile and dissolves, and be diluted to
Scale, shakes up, and as test sample solution, carries out efficient liquid phase chromatographic analysis under above-mentioned chromatographic condition, records chromatogram, knot
Fruit sees accompanying drawing 2.
Each composition result:
| Retention time (min) | Composition | Content (%) |
| 11.361 | TRIBROMOBISPHENOL A | 0.12 |
| 14.278 | TETRABROMOBISPHENOL A | 99.45 |
| 22.838 | Other | 0.43 |
Claims (3)
1. the separation of a tetrabromobisphenol A composition and analysis determining method, it is characterised in that: use high performance liquid chromatograph, use
Octadecyl silane is the chromatographic column of filler, with the mixture of acetonitrile and water for flowing phase, uses the side of gradient elution
Composition in tetrabromobisphenol A sample solution is detected by method, wherein: described chromatographic column use specification be 250mm ×
4.6mm, the chromatographic column of 5 μm；During detection, the column temperature of chromatographic column is 30 DEG C, and wavelength is 254nm；Use gradient elution method be
In 0～30min, acetonitrile: the volume ratio of water is from 50:50 even variation to 0:100, and flow rate of mobile phase is 0.8ml/min；Tetrabromo is double
The concentration of phenol A sample solution is 0.01g/ml acetonitrile, and sampling volume is 20 μ l.
The separation of tetrabromobisphenol A composition the most according to claim 1 and analysis determining method, it is characterised in that: described
In the mixture of acetonitrile and water, both volume ratios are acetonitrile: water=50:50～0:100.
The separation of tetrabromobisphenol A composition the most according to claim 1 and analysis determining method, it is characterised in that: described
High performance liquid chromatograph is Agilent 1100.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103901140B (en) * | 2014-04-28 | 2015-10-21 | 中国环境科学研究院 | A kind of pre-treating method analyzed for tetrabromobisphenol A in ight soil after biology contamination |
| CN103901139B (en) * | 2014-04-28 | 2016-04-20 | 中国环境科学研究院 | A kind of pre-treating method analyzed for tetrabromobisphenol A in biological urine |
| CN103901143B (en) * | 2014-04-28 | 2016-04-20 | 中国环境科学研究院 | A kind of pre-treating method analyzed for tetrabromobisphenol A in a small amount of biological anteserum |
| CN107091899B (en) * | 2017-06-05 | 2019-07-02 | 环境保护部华南环境科学研究所 | The rapid assay methods of tetrabromobisphenol A in a kind of environment water |
| CN114527215B (en) * | 2022-04-08 | 2024-04-09 | 江苏康达检测技术股份有限公司 | Method for detecting environmental endocrine disruptors for solid waste |
| CN115508469B (en) * | 2022-09-21 | 2023-05-26 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | High-resolution detection method for tetrabromobisphenol A in milk powder |
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Non-Patent Citations (6)
| Title |
|---|
| LC-ESI-MS-MS method for the analysis of tetrabromobisphenol A in sediment and sewage sludge;Richard Saint-Louis等;《Analyst》;20040706;第129卷;724-730 * |
| Richard Saint-Louis等.LC-ESI-MS-MS method for the analysis of tetrabromobisphenol A in sediment and sewage sludge.《Analyst》.2004,第129卷724-730. * |
| 液相色谱-质谱法同时测定塑料制品中的双酚A和四溴双酚A;黄少婵等;《色谱》;20100930;第28卷(第9期);863-866 * |
| 肖全伟.酚类环境雌激素的色谱测定方法及其应用研究.《中国优秀博硕士学位论文全文数据库（博士） 医药卫生科技辑》.2007,(第3期),第二部分第2节. * |
| 酚类环境雌激素的色谱测定方法及其应用研究;肖全伟;《中国优秀博硕士学位论文全文数据库（博士） 医药卫生科技辑》;20070315(第3期);第二部分第2节 * |
| 黄少婵等.液相色谱-质谱法同时测定塑料制品中的双酚A和四溴双酚A.《色谱》.2010,第28卷(第9期),863-866. * |
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