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Method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products

A technology for alkylphenol polyoxyethylene ether and chemical products is applied in the field of quantitative determination of alkylphenol polyoxyethylene ether in daily chemical products, which can solve the problem of large difference in molecular weight, qualitative deviation, and inconsistent relative abundance of fragment ions and other problems, to achieve the effect of simple pre-processing, high accuracy, good economic and social benefits

Active Publication Date: 2013-06-26
GUANGZHOU QUALITY SUPERVISION & TESTING INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since alkylphenol polyoxyethylene ethers have different forms of compounds with different degrees of polymerization in different products, the peak time of different polymerization degrees is different, and the span of the peak time is relatively large, which makes it impossible to use the peak time Quantitative judgment of alkylphenol polyoxyethylene ether
Moreover, due to the large difference in the molecular weight of alkylphenol ethoxylates with different degrees of polymerization, if the compounds of various degrees of polymerization are not effectively separated, only UV or fluorescence is used for quantification, which will lead to serious quantitative errors
The qualitative and quantitative use of mass spectrometry may also cause inconsistent relative abundances of fragment ions due to the existence of isomers. In addition, the abundance of various mass spectrometry ion adducts (M+NH4, M+Na, M+K) is affected by Systematic influence is large and may also lead to qualitative bias

Method used

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  • Method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products
  • Method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products
  • Method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Nonylphenol polyoxyethylene ether (NP) in the laundry liquid sample of embodiment 1 n EO) and octylphenol ethoxylates (OP n Determination of EO) content

[0042] 1. Preparation of samples

[0043] Accurately weigh 0.5g (accurate to 0.001g) of laundry detergent sample, put it into a 10mL stoppered centrifuge tube, add about 9mL of acetonitrile aqueous solution (8:2, v / v), mix on a vortex oscillator to disperse the sample, Place in an ultrasonic generator for extraction for 15 minutes, and dilute to the mark with aqueous acetonitrile. The extract was centrifuged at 15000r / min for 5min and filtered with a 0.45μm membrane to obtain the test sample.

[0044]Pipette nonylphenol ethoxylates (Nippon Hayashi Junyaku, 100 μg / mL) and octylphenol ethoxylates (Nippon Hayashi Junyaku, 100 μg / mL), and use acetonitrile aqueous solution as a solvent to dissolve the above nonyl Dilute phenol ethoxylates and octylphenol ethoxylates to 2.0mg / L, 4.0mg / L, 10.0mg / L, 20.0mg / L, 50.0mg / L to ...

Embodiment 2

[0083] Example 2 Nonylphenol polyoxyethylene ether (NP) in cream cosmetic sample 1 n EO) and octylphenol ethoxylates (OP n Determination of EO) content

[0084] 1. Preparation of samples

[0085] Same as Example 1

[0086] 2. Determination by HPLC

[0087] With embodiment 1, obtain test sample chromatogram, as Figure 4 Shown, and judging from the peak time that the added substance is NPEO.

[0088] 3. Quantitative calculation

[0089] 3.1 Calculation of fluorescence molar absorption coefficient (ε)

[0090] Same as the fluorescence molar absorption coefficient ε obtained in Table 2 in Example 1.

[0091] 3.2 Calculate the average molecular weight (M 平均 )

[0092] In this case, under the same instrument and research conditions, taking cream cosmetic 1 as a sample, the following Figure 4 Shown liquid chromatogram, its average molecular weight calculating method is with embodiment 1, specifically following table 5:

[0093] Table 5 Nonylphenol polyoxyethylene ether (...

Embodiment 3

[0100] Example 3 Nonylphenol polyoxyethylene ether (NP) in cream cosmetic sample 2 n EO) and octylphenol ethoxylates (OP n Determination of EO) content

[0101] 1. Preparation of samples

[0102] Same as Example 1

[0103] 2. Determination by HPLC

[0104] With embodiment 1, obtain test sample chromatogram, as Figure 5 Shown, and judging from the peak time that the added substance is OPEO.

[0105] 3. Quantitative calculation

[0106] 3.1 Calculation of fluorescence molar absorption coefficient (ε)

[0107] Same as the fluorescence molar absorption coefficient ε obtained in Table 2 in Example 1.

[0108] 3.2 Calculate the average molecular weight (M 平均 )

[0109] In this case, under the same instrument and research conditions, taking cream cosmetic 2 as a sample, the following Figure 5 Shown liquid chromatogram, its average molecular weight calculating method is the same as embodiment 1, specifically following table 6:

[0110] Table 6 Octylphenol polyoxyethylene ...

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Abstract

The invention discloses a method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products, belonging to the technical field of analysis of daily chemical products. The method comprises the following steps of: preparing test samples, detecting the test samples via a high performance liquid chromatography, separating substances to be detected through a method for hybridizing a reversed-phase C18 column with an HILIC (Hydrophilic Interaction Liquid Chromatography) silica gel chromatography column, and quantitatively detecting the content of the alkylphenol polyoxyethylene in a daily chemical product through a fluorescence molar absorption coefficient method. Due to the method disclosed by the invention, the technical problem of great quantification errors of the alkylphenol polyoxyethylene can be effectively solved, and thus the method is very suitable for precise quantification and batch detection on the alkylphenol polyoxyethylene in the daily chemical products, provides important technical support for the mass control and the safety monitoring of the daily chemical products, and has good economic and social benefits.

Description

technical field [0001] The invention relates to the field of analysis of daily chemical products, in particular to a method for quantitatively measuring alkylphenol polyoxyethylene ethers in daily chemical products. Background technique [0002] Alkylphenol polyoxyethylene ether (APEO S ) is a kind of non-ionic surfactant prepared by the reaction of alkylphenol and ethylene oxide. It is widely used in daily chemical industry because of its good wetting, penetrating, emulsifying, dispersing, solubilizing and washing functions. and other industries. According to statistics, APEO S Use nonylphenol polyoxyethylene ether (NP n EO) or octylphenol ethoxylates (OP n EO) mainly, the two together account for more than 95% of the total, and one of them is often added when used. However, due to APEO S It has ecotoxicity, poor biodegradability and may cause environmental endocrine disruption problems. EU Directive 2003 / 53 / EC restricts its use in chemicals and their preparations to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 席绍峰李慧勇谭建华
Owner GUANGZHOU QUALITY SUPERVISION & TESTING INST
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