Method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine on basis of low-temperature frozen extraction technology

An extraction technology and a technology for polycyclic aromatic hydrocarbons, which are applied in the field of detecting unmetabolized polycyclic aromatic hydrocarbons in urine based on low temperature freezing extraction technology, can solve the problem of high technical cost, achieve high selectivity and sensitivity, improve the recovery rate of standard addition, The effect of improving the bonding rate

Active Publication Date: 2019-11-12
SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The extraction methods of non-metabolized PAHs in urine are solid-phase microextraction, which is relatively expensive

Method used

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  • Method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine on basis of low-temperature frozen extraction technology
  • Method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine on basis of low-temperature frozen extraction technology
  • Method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine on basis of low-temperature frozen extraction technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Collection of samples

[0030] Urine samples were collected from fourth-grade primary school students, and urine samples were collected from children's morning urine for three consecutive days.

[0031] (2) Experimental materials and instruments

[0032] Instruments: gas chromatography-triple quadrupole tandem mass spectrometer, nitrogen blowing instrument (ETEL4MG-2200), vortex instrument (SIVortex-2), centrifuge (DT5-2), aerosol spray generator (TSI 3079), CO2 pump.

[0033] Materials: acetonitrile, n-hexane, toluene, nonane, liquid carbon dioxide, trimethylchlorosilane, di-tert-butyl dicarbonate, sodium chloride, potassium chloride, 16 deuterated polycyclic aromatic hydrocarbon isotope standard solutions, etc., such as Unless otherwise specified, the reagents in this example are all commercially available products.

[0034] (3) Experimental method

[0035] This embodiment mainly adopts the method of detecting non-metabolized polycyclic aromatic hydrocarbons in ...

Embodiment 2

[0046] This embodiment mainly adopts the method of detecting non-metabolized polycyclic aromatic hydrocarbons in urine by low-temperature freezing extraction technology, which includes the following steps;

[0047] S1: Mix 10ml of urine specimen with 5ml of acetic acid buffer, add 1ml of 16 kinds of deuterated polycyclic aromatic hydrocarbon isotope standard solution (purchased from Wuhan Ruichen Standard Material Technology Co., Ltd.) as a recovery rate indicator, and obtain the sample to be tested; acetic acid The buffer can also be replaced by ammonium acetate buffer at a concentration of 1mol / L.

[0048] S2: adding a certain amount of pretreatment agent to the sample to be tested, using the electrode stirring head to stir at 25° C. for 3 minutes, and using the electrode to excite the pretreatment agent to pretreat the sample to be tested to obtain a pretreated urine sample; The pretreatment agent is composed of trimethylchlorosilane, di-tert-butyl dicarbonate, sodium chlor...

Embodiment 3

[0057] This embodiment mainly adopts the method of detecting non-metabolized polycyclic aromatic hydrocarbons in urine by low-temperature freezing extraction technology, which includes the following steps;

[0058] S1: Mix 10ml of urine specimen with 5ml of acetic acid buffer, add 1ml of 16 kinds of deuterated polycyclic aromatic hydrocarbon isotope standard solution (purchased from Wuhan Ruichen Standard Material Technology Co., Ltd.) as a recovery rate indicator, and obtain the sample to be tested; acetic acid The buffer can also be replaced by ammonium acetate buffer at a concentration of 1mol / L.

[0059] S2: adding a certain amount of pretreatment agent to the sample to be tested, using an electrode stirring head to stir at 22° C. for 5 minutes, and using the electrode to excite the pretreatment agent to pretreat the sample to be tested to obtain a pretreated urine sample; The pretreatment agent is composed of trimethylchlorosilane, di-tert-butyl dicarbonate, sodium chlori...

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Abstract

The invention discloses a method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine on the basis of a low-temperature frozen extraction technology. According to the method, a preprocessing agent is added into a to-be-detected sample, and pulse stimulation is carried out by utilizing an asymmetric phase current so as to improve a binding rate of an indicator and a target object;then after an extraction agent is atomized, the extraction agent is blown into the to-be-extracted sample along with pressurized CO2 gas, and simultaneously, ultrasonic cavitation is carried out, so as to shorten low-temperature extraction time and improve extraction efficiency; then freezing is carried out to remove an extraction phase; and finally, the unmetabolized polycyclic aromatic hydrocarbons in the urine are detected by utilizing a gas chromatography-triple quadrupole tandem mass spectrometry method. According to the invention, interference of various matrices in the sample can be effectively eliminated and analyzed, and sensitivity and reliability are higher.

Description

technical field [0001] The invention belongs to the technical field of environmental detection, and in particular relates to a method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine based on low-temperature freezing extraction technology. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are a class of persistent organic pollutants that exist widely. Due to their carcinogenicity, triple effects, and widespread distribution around the world, the potential harm of PAHs to human health has become an environmental pollution issue that is widely concerned by countries all over the world. The assessment of human exposure level is an important basic scientific data for PAHs health risk assessment. Studies have shown that the determination of PAHs metabolites in urine is usually closely related to PAHs exposure, so traditional research has always regarded hydroxyl PAHs as an important biomarker to reflect the exposure load of human PAHs. In...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14G01N30/04G01N30/88
CPCG01N30/02G01N30/72G01N30/06G01N30/14G01N30/04G01N30/88G01N2030/062G01N2030/146G01N2030/045G01N2030/8813
Inventor 赵波黎玉清李彦希金梦潘浪古丽娜谢丹平
Owner SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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