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Method for detecting 4-nonylphenol ethoxylate through ultra-high-performance liquid chromatography-PDA combination

An ethoxylate, ultra-high performance liquid phase technology, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as lack of detection methods

Inactive Publication Date: 2019-06-14
GREE ELECTRIC APPLIANCES INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the difficulty of supervision and the lack of detection methods, there are few domestic researches on the determination of NPEO

Method used

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  • Method for detecting 4-nonylphenol ethoxylate through ultra-high-performance liquid chromatography-PDA combination
  • Method for detecting 4-nonylphenol ethoxylate through ultra-high-performance liquid chromatography-PDA combination
  • Method for detecting 4-nonylphenol ethoxylate through ultra-high-performance liquid chromatography-PDA combination

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Experimental program
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Embodiment 1

[0034] Embodiment 1: sample preparation

[0035] In the embodiment of the present application, methanol is selected as the extraction solvent to perform ultrasonic extraction on the same sample, and the extraction temperature is kept at 25°C for 5min, 15min, 30min, 45min, 60min, and 120min respectively. The test results show that as the extraction time increases, the measured value also increases Increased accordingly, but after 30 minutes, the measured value basically stopped increasing. Therefore, this experiment chooses the ultrasonic extraction time as 30min, which is the most energy-saving and efficient ultrasonic extraction time.

[0036] The specific preparation method is: accurately weigh 0.1g sample (accurate to 0.01g), add it into a 10ml test tube, then add 10ml methanol, and perform ultrasonic extraction at 25°C for 30 minutes in an ultrasonic cleaner. After filtering through a 0.22μm filter membrane, it is used for UPLC-PDA injection. Carry out a blank experiment...

Embodiment 2

[0037] Embodiment 2: determination of chromatographic conditions

[0038] Chromatographic column selection: the examples of this application compare the following three chromatographic columns

[0039] JADE- Amide column, 150mm×4.6mm(id.), 5μm;

[0040] Agilent ZorAX SB-CN column, 150mm×4.6mm(id.), 1.7μm;

[0041] C18 chromatographic column, 186002350 150mm×2.1mm (id.), 1.7μm chromatographic column.

[0042] It is found through experimental analysis that C18, 186002350 150mm×2.1mm (id.), 1.7μm chromatographic column is more suitable for 4-nonylphenol ethoxylate, while Amide column hardly retains 4-nonylphenol ethoxylate , therefore, a C18, 186002350 150mm×2.1mm (id.), 1.7μm chromatographic column is used.

[0043] Mobile phase selection: Methanol-water, acetonitrile-water, methanol-isopropanol were used to investigate the influence on separation and ionization respectively. The results show that the chromatographic peak shape, resolution and ionization effect are better ...

Embodiment 3

[0047] Embodiment 3: the drawing of standard curve

[0048] According to the method described in embodiment 1, configure a specific concentration of 4-nonylphenol ethoxylate stock solution with a volumetric flask, add methanol and dilute it into a series of standard solutions of different concentrations respectively, and the standard solutions are configured with 4 different concentrations in total, according to The assay condition after this method optimization, the series standard solution of 4-nonylphenol ethoxylate under four concentrations is detected, and the detection result is as follows figure 1 Shown, then take the 4-nonylphenol ethoxylate concentration as the abscissa, the unit is expressed in mg / L, and take the peak area corresponding to the 4-nonylphenol ethoxylate as the ordinate to draw a standard curve to obtain a linear equations and correlation coefficients, standard curves such as figure 2 so. The linear equation is Y=3220.48X-248.313, and the correlatio...

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Abstract

The application relates to the technical field of the material detection, and specifically relates to a method for detecting 4-nonylphenol ethoxylate through ultra-high-performance liquid chromatography-PDA combination. The method comprises the following steps: preparing a to-be-detected sample solution and a 4-nonylphenol ethoxylate standard solution for the sample feeding of the ultra-high-performance liquid chromatography-PDA, wherein the chromatographic column selects a C18 column in the specification of 150mm*2.1mm, and 1.7 micron, the moving phase selects methanol-isopropanol solution, the volume ratio is 93: 7, the flow velocity is 0.2mL / min, and the detection wavelength is 275.45nm; and computing the content of the 4-nonylphenol ethoxylate. The experimental principle of the methodis to ultrasonically extract a sample in a solvent environment, the residual NPEO is extracted, and is separated and purified when passing through the chromatographic column; the specific wavelength is absorbed when passing through a PDA detector, the content thereof and the absorbance are in direct proportion when the 4-nonylphenol ethoxylate is in low concentration according to the Lamberbier'slaw. The method has the features of being efficient, fast, accurate and reliable, and high in sensitivity, and the requirement of the overseas law detection limit can be satisfied.

Description

technical field [0001] The present application relates to the technical field of material detection, in particular to a method for detecting 4-nonylphenol ethoxylates by ultra-high performance liquid chromatography-PDA. Background technique [0002] 4-Nonylphenol ethoxylate, also known as isononylphenyl polyethylene glycol, CAS No. 37205-87-1, English name Poly(oxy-1,2-ethanediyl), hereinafter referred to as NPEO. NPEO is a common nonionic surfactant, which reacts in the natural environment to lose ethoxylates to produce nonylphenols. NPEO is widely used in printing and dyeing and cleaning processes in the textile industry, and can also be used as a surfactant and cleaning agent. Because its chemical structure is similar to human estrogen, it will interfere with the normal operation of endocrine after entering the human body, and can promote the proliferation of breast cancer cells. It is a carcinogen, and its biological toxicity has been highly concerned. For the first ti...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 顾然窦晓文廖永慷苗旭吴泽滔陆松邓智欧毓迎吕锦銮
Owner GREE ELECTRIC APPLIANCES INC
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