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Detection method of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt

A technology for methoxybenzophenone and a detection method, which is applied in the field of high performance liquid chromatography-tandem quadrupole mass spectrometry detection, can solve the problem of unsuitable textiles, difficult 2-hydroxy-4-methoxybenzophenone -5-sulfonic acid qualitative confirmation and other issues, to achieve the effect of easy operation, ensuring accuracy, and improving detection sensitivity

Active Publication Date: 2022-08-09
福建省纤维检验局
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although this method can be used for the determination of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid in sunscreen, on the one hand, cloud point extraction is a liquid-liquid extraction technique, which is not suitable for textiles ; On the other hand, photometric method is difficult to carry out accurate qualitative confirmation to 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid, there are certain limitations in the actual application process
[0005] At present, there is no domestic research report on the detection method of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt in textiles by high performance liquid chromatography-tandem quadrupole mass spectrometry

Method used

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  • Detection method of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt
  • Detection method of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt
  • Detection method of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1), prepare the sample solution to be tested:

[0059] Take a representative textile sample, cut it into pieces below 5mm × 5mm, and mix it as a sample. Weigh 1.0g of sample (accurate to 0.01g), place it in an extractor with a plug, add 25mL of methanol as an extractant, seal it and shake it well, place it in an ultrasonic generator, and extract it ultrasonically at 30°C for 20min. 0.22μm organic microporous membrane filter into the sample bottle;

[0060] The material-to-liquid ratio of the sample to the extractant is: 1 g of sample: 25 mL of extractant.

[0061] 2), prepare standard solution:

[0062] (1) Weigh 0.0115g of molecular formula as C respectively 14 H 12 O 6 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid of S or 0.0102g molecular formula is C 14 H 11 O 6 SNa's 2-hydroxy-4-methoxybenzophenone-5-sodium sulfonate standard substance was dissolved in methanol and made up to volume to configure a standard stock solution with a concentration of 1000 mg / L;...

experiment example

[0105] Experimental Example: Recovery Experiment and Precision Experiment

[0106] Add 1.25mg / kg, 2.5mg / kg, 12.5mg / kg of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid or 2-hydroxy-4-methoxyl The standard solution of sodium benzophenone-5-sulfonate was repeated 6 times for each group according to the above-mentioned pretreatment and analysis methods, and the average recovery was obtained by measurement and calculation, and the precision was calculated by relative standard deviation (RSD), as shown in Table 5.

[0107] Table 5 Spike recovery and precision (n=6)

[0108]

Embodiment 2

[0110] It differs from Example 1 as follows (the rest are equivalent to Example 1):

[0111] 1), prepare the sample solution to be tested:

[0112] Take a representative textile sample, cut it into pieces below 5mm × 5mm, and mix it as a sample. Weigh 1.0g sample (accurate to 0.01g), place it in a plugged extractor, accurately add 30mL extractant methanol, seal it and shake it well, place it in an ultrasonic generator, extract ultrasonically at 30°C for 30min, and extract the extract with 0.22μm organic microporous membrane filter into the sample bottle;

[0113] The material-to-liquid ratio of the sample to the extractant is: 1 g of sample: 30 mL of extractant.

[0114] 2), prepare standard solution:

[0115] (1) Weigh 0.0115g of molecular formula as C respectively 14 H 12 O 6 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid of S or 0.0102g molecular formula is C 14 H 11 O 6 SNa's 2-hydroxy-4-methoxybenzophenone-5-sodium sulfonate standard substance was dissolved in m...

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Abstract

The invention discloses a detection method suitable for 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt in textiles. The invention adopts an ultrasonic extraction method and uses a suitable extraction agent for airtight extraction. 2-Hydroxy-4-Methoxybenzophenone-5-sulfonic acid and its sodium salt in textile samples, the two substances can be extracted more thoroughly, and then using high performance liquid chromatography-tandem quadrupole mass spectrometer , Double ion pair negative ion monitoring for qualitative and quantitative analysis and determination of the extract, liquid chromatography conditions using C18 chromatographic column, using gradient elution mode to effectively separate the target from other components within 12 minutes. The method is easy to operate, high sensitivity, accurate and reliable, and is very advanced and innovative.

Description

technical field [0001] The invention relates to a high performance liquid chromatography-tandem quadrupole mass spectrometry detection method suitable for 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its sodium salt in textiles. Background technique [0002] In view of the harmfulness of ultraviolet light to the human body, the anti-ultraviolet radiation performance of textiles has attracted more and more attention. 2-Hydroxy-4-methoxybenzophenone-5-sulfonic acid (CAS: 4065-45-6), 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid sodium (CAS: 6628-37-1) is widely used in various industrial and consumer products, such as textiles, plastics, cosmetics, paints, pigments, coatings and other fields due to its wide effective absorption wavelength range, good compatibility and good stability. However, studies have shown that it has estrogenic effects and induces the secretion of pS2 protein by breast cancer cells. Large doses or long-term exposure will cause skin toxicity an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14G01N30/34G01N30/04
CPCG01N30/02G01N30/04G01N30/06G01N30/14G01N30/34G01N30/72G01N2030/146G01N2030/062G01N2030/047
Inventor 朱峰裴德君林金美林丽云柯萍英林嘉欢陈姗影杨瑜榕滕牧潘行星
Owner 福建省纤维检验局