Method for determining trace chlorophenol endocrine disruptor in water

A technology for endocrine disruptors and chlorophenols, which is used in measurement devices, material separation, and analysis of materials, etc., to achieve the effects of short phase separation time, less emulsification, and good precision.

Inactive Publication Date: 2012-11-07
JILIN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since 2003, after Rogers et al. discovered the ionic liquid two-phase system, the system has successfully extracted and separated testosterone, epitestosterone, opioid, protein, roxithromycin and other substances, and used the ionic liquid two-phase system to extract and separate chlorophenol Endocrine disruptors have not been reported yet

Method used

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  • Method for determining trace chlorophenol endocrine disruptor in water
  • Method for determining trace chlorophenol endocrine disruptor in water
  • Method for determining trace chlorophenol endocrine disruptor in water

Examples

Experimental program
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Embodiment Construction

[0020] Step 1: Accurately pipette 8mL water sample (tap water, lake water or industrial wastewater that may contain 4-DCP, 2,6-DCP or / and 4-CP) into a 20mL colorimetric tube;

[0021] Step 2: Add 5gNaH 2 PO 4 , and use Na 2 HPO 4 -H 3 PO 4 Buffer solution to adjust the pH value of the test solution to 4, add twice distilled water to make the volume to 10mL, add [Bmim]BF 4 2.0mL, extract and shake for 4min;

[0022] Step 3: Stand still for 10 minutes, centrifuge at 3000r / min for 5 minutes, after the layering is clear, suck out the ionic liquid phase, automatically inject 10 μL, and use high performance liquid chromatography to determine the content of chlorophenol endocrine disruptors.

[0023] The chromatographic condition of described high performance liquid chromatography:

[0024] Using Kromasil100C 18 Chromatographic column (150mm×4.6mm×μm), mobile phase is acetonitrile-water (60:40, V / V) solution, flow rate is 1.0mL / min, column temperature is 30°C, column pressure...

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Abstract

The invention relates to a chlorophenol compound measuring method, specifically to a method for determining a trace chlorophenol endocrine disruptor in water. The method comprises the following steps of: adding NaH2PO4 phase separation salt, adding a Na2HPO4-H3PO4 buffer solution to adjust pH value of the solution, adding a [Bmim]BF4 hydrophilic ionic liquid for extraction separation, separating by a centrifuge, taking an ionic liquid phase, and finally determining the content of the chlorophenol endocrine disruptor through HPLC. According to the invention, the ionic liquid is used as an extractant, NaH2PO4 is used as the phase separation salt, and the trace chlorophenol endocrine disruptor in water is determined by the utilization of the ionic liquid aqueous biphasic extraction-high performance liquid chromatography (HPLC) method, which has advantages of short phase separation time, no easy emulsification during the extraction process, nontoxicity, no pollution and the like in comparison with polymer aqueous biphasic extraction. The method provided by the invention has high accuracy and good precision.

Description

technical field [0001] The invention relates to a method for measuring chlorophenol compounds, in particular to a method for measuring trace amounts of chlorophenol endocrine disruptors in water. Background technique [0002] Chlorophenols (CPs) are chemical raw materials commonly used in pesticides, preservatives and herbicides. They are highly toxic and difficult to biodegrade. They can be enriched in organisms through the food chain and have carcinogenic and teratogenic properties. , mutagenic effect, is the priority pollutants controlled by the environmental protection departments of various countries. [0003] At present, the methods for the determination of chlorophenol endocrine disruptors mainly include high-performance liquid chromatography (HPLC), ultraviolet spectrophotometry, gas chromatography (GC) and gas chromatography-mass spectrometry, etc. Pre-separation and enrichment are required. The commonly used pretreatment methods mainly include solvent extraction, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 王良马春宏姜大雨朱红
Owner JILIN NORMAL UNIV
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