Detection method of 2-phenylbenzimidazole-5-sulfonic acid in soil

A technology of phenylbenzimidazole and detection method, applied in the field of environmental sample detection, can solve the problems of PBSA detection method research and almost blank research on content level, and achieve the effects of similar retention time, increased recovery rate, and offset error.

Active Publication Date: 2017-10-27
山东西格玛检测技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the research on PBSA mainly focuses on the content level in cosmetics and products, and the research on the degradation mechanism in the water environment, but the research on the detection method and content level of PBSA in soil is almost blank

Method used

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  • Detection method of 2-phenylbenzimidazole-5-sulfonic acid in soil
  • Detection method of 2-phenylbenzimidazole-5-sulfonic acid in soil
  • Detection method of 2-phenylbenzimidazole-5-sulfonic acid in soil

Examples

Experimental program
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Effect test

Embodiment 1

[0039] (1) Ultrasonic extraction

[0040] 100 g of soil samples were collected, freeze-dried and removed larger impurities such as stones and plant tissues, and ground through a 0.90 mm sieve. Weigh 5g of soil sample into a centrifuge tube with a cover, add 100μL of 1mg / L internal standard 2-methyl-4-chloropentyloxypropionic acid working solution dropwise, and wait for the solvent to evaporate; add 10mL of ethyl acetate and formic acid to mix Solvent (volume ratio 50:1), tighten the cap, vortex mix for 30s, ultrasonically extract for 15min, centrifuge at 2500rpm for 15min, draw the supernatant into a pear-shaped flask, repeat the extraction twice, combine the extracts into a pear-shaped flask, Rotary evaporate to dryness at 45°C.

[0041] (2) Silica gel column purification

[0042] Put a small amount of glass wool at the bottom of the glass chromatography column, add 1g of silica gel and 0.5g of anhydrous sodium sulfate in sequence, tap the flat surface of the glass column, ...

Embodiment 2

[0058] (1) Ultrasonic extraction

[0059] 100 g of soil samples were collected, freeze-dried and removed larger impurities such as stones and plant tissues, and ground through a 0.90 mm sieve. Weigh 10g of soil sample into a centrifuge tube with a cover, add 100μL of 1mg / L internal standard 2-methyl-4-chloropentyloxypropionic acid working solution dropwise, and wait for the solvent to evaporate; add 10mL of ethyl acetate and formic acid to mix Solvent (volume ratio 100:1), tighten the cap, vortex mix for 30s, ultrasonically extract for 15min, centrifuge at 2500rpm for 15min, draw the supernatant into a pear-shaped flask, repeat the extraction twice, combine the extracts into a pear-shaped flask, Rotary evaporate to dryness at 45°C.

[0060] (2) Silica gel column purification

[0061] Put a small amount of glass wool at the bottom of the glass chromatography column, add 1g of silica gel and 0.5g of anhydrous sodium sulfate in sequence, tap the flat surface of the glass column...

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Abstract

The invention belongs to the field of environmental sample detection, and particularly relates to a detection method of 2-phenylbenzimidazole-5-sulfonic acid (PBSA) in soil. At present, studies on PBSA mainly focus on content levels in cosmetics and products, and a degradation mechanism in a water environment; but, almost no study focuses on a detection method and a content level of PBSA in the soil; therefore, in order to learn a concentration level and an environmental behavior of PBSA in a soil environment, an efficient, quick and highly sensitive analysis method is required to be established for qualitative and quantitative detection of a trace amount of 2-phenylbenzimidazole-5-sulfonic acid in the soil; and the invention aims at providing an analysis and detection method of PBSA in the soil, in particular to an analysis method using ultrasonic extraction, silica gel chromatographic column purification and high-performance liquid chromatograph-mass spectrometer detection.

Description

1. Technical field [0001] The invention belongs to the field of environmental sample detection, in particular to a method for detecting 2-phenylbenzimidazole-5-sulfonic acid in soil. 2. Background technology [0002] In recent years, since whitening and UV protection are paid more and more attention to, sunscreens are used more and more frequently. After the sunscreen is used on people's skin, it will directly enter the environment along with people's activities, or first enter the urban sewage treatment system, and then enter the environment with the discharge of sludge and sewage. Many studies have shown that sunscreen can be detected in many water environments. As a new type of pollutant, it has received the attention of environmental protection departments and environmental researchers. Several studies have shown that organic sunscreens are endocrine disruptive and bioaccumulative in the environment, making them potentially harmful to the environment. [0003] 2-Phenyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 奈世杰李焕明姜红牟文超卢燕华刘安栋奈欣慧杨素云胡睿刘子叶王鹏程
Owner 山东西格玛检测技术服务有限公司
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