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High performance liquid chromatography detection method of tris(nonylphenol)phosphite

A high-performance liquid chromatography and phosphite technology, applied in the field of high-performance liquid chromatography detection of triphosphite, can solve the problem that antioxidant TNPP is weak in hydrophilicity, antioxidant TNPP is easily oxidized, and cannot achieve accurate quantitative analysis. and other problems, to achieve the effect of increasing solution stability and method accuracy, improving detection sensitivity, and good recovery rate.

Active Publication Date: 2018-08-14
上海市食品药品包装材料测试所
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing methods for analyzing antioxidants have the following technical defects when they are used to analyze the antioxidant TNPP: (1) the antioxidant TNPP is easily oxidized, and has poor stability during extraction tests and sample processing. (2) The compatibility research of packaging materials often uses a variety of extraction media, and the existing methods cannot be applied to all media; (3) The hydrophilicity of the antioxidant TNPP is weak, and it can be used in Retention on reverse chromatographic column is stronger, if adopt the analysis method of general antioxidant, not only analysis time is long, and sensitivity is low; (4) pretreatment operation is complicated in the existing antioxidant analysis method, or used More toxic organic solvents such as methyl chloride, thus posing a potential risk to the health of operators
[0004] It can be seen that the analytical method provided by the prior art shows many technical defects in the determination of antioxidant TNPP, so it is urgent to provide a new analytical method, which is applicable to the content determination of antioxidant TNPP in various media

Method used

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  • High performance liquid chromatography detection method of tris(nonylphenol)phosphite

Examples

Experimental program
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Embodiment 1

[0022] HPLC conditions include: Agilent 1290 high performance liquid chromatograph, equipped with UV detector, binary pump and autosampler; chromatographic column is Agilent Eclipse XDB-C8 (4.6×150mm, 5μm); mobile phase: acetonitrile-isopropanol (Volume ratio 90:10); Flow rate: 1ml / min; Analysis time: 18 minutes; Column temperature: 35°C; Detection wavelength: 220nm; Injection volume: 20μl.

[0023] Accurately weigh the appropriate amount of tris(nonylphenol) phosphite (antioxidant TNPP) reference substance, dissolve it in dichloromethane, prepare a 0.2mg / ml control stock solution, and dilute it with acetonitrile to the corresponding concentration as needed The control solution was used to determine the detection limit of the antioxidant TNPP content in water, 0.9% sodium chloride injection, pH 3.5 buffer, pH 8.0 buffer, and 15% ethanol (a total of five extraction media). Limit of quantification, linearity, repeatability, recovery and stability.

[0024] Mix ethyl acetate and tert...

Embodiment 2

[0027] HPLC conditions include: Agilent 1290 high performance liquid chromatograph, equipped with UV detector, binary pump and autosampler; chromatographic column is Agilent Eclipse XDB-C8 (4.6×150mm, 5μm); mobile phase: acetonitrile-isopropanol (Volume ratio 90:10); Flow rate: 1ml / min; Analysis time: 18 minutes; Column temperature: 35°C; Detection wavelength: 220nm; Injection volume: 20μl.

[0028] Accurately weigh an appropriate amount of tris(nonylphenol) phosphite (antioxidant TNPP) reference substance, dissolve it in dichloromethane, prepare a 0.2mg / ml control stock solution, and dilute it with isopropanol as needed for corresponding use Concentration of the control solution; accurately weigh 0.9ml of the control solution, place it in a liquid injection vial, precisely add 100μl of the derivatization reagent prepared in "Example 1", cover and mix well, then take 20μl and inject it into the high performance liquid chromatograph In, record the chromatogram to investigate the d...

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Abstract

The invention provides a high performance liquid chromatography detection method of tris(nonylphenol)phosphite. The method comprises the following steps of uniformly mixing a tris(nonylphenol)phosphite to be detected with tert-butyl hydroperoxide solution; performing pre-column derivatization to produce a derivative solution; performing sampling in the derivative solution; feeding samples to an HPLC system; performing high performance liquid chromatography detection under the high performance liquid chromatography detection conditions of using a reverse phase chromatographic column, using thedetection wavelength of the ultraviolet detector to be 220+ / -2nm and forming the flowing phase by acetonitrile and isopropanol, wherein the volume percentage of acetonitrile is 80 to 100 percent; performing isocratic elution. By using the detection method, antioxidants TNPP are oxidized into more stable organic phosphate by phosphite ester, so that the solution stability and the method accuracy can be improved; the analysis time is simultaneously reduced; the color spectrum peak shapes are improved; the detection sensitivity is improved, so that the requirement of quantitative analysis in medicine and food packaging material compatibility study can be met; wide application prospects are realized.

Description

Technical field [0001] The invention relates to the technical field of instrument analysis, in particular to a high performance liquid chromatography detection method for tris(nonylphenol) phosphite. Background technique [0002] Tris (nonylphenol) phosphite (antioxidant 1178 or TNPP for short, CAS NO.: 26523-78-4) is a kind of phosphite antioxidant, which can be used in a variety of polymers (such as polyethylene , Styrene butadiene rubber and polyvinyl chloride, etc.), the addition amount is mostly between 0.05% and 3%. As the antioxidant TNPP is widely used in food contact packaging, the risk assessment report issued by the Directorate-General of Health and Consumer Protection of the European Commission pointed out that the daily intake of TNPP for ordinary consumers is about 0.0337 mg. TNPP has low water solubility (0.6mg·L -1 ), TNPP has low oral toxicity. Animal toxicology test data show that the oral LD50 of rats is 19500mg·kg -1 . However, when polymer materials are us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 刘小慧王蓉佳张芳芳
Owner 上海市食品药品包装材料测试所
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