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Method for detecting semi-volatile organic compounds in blood

A semi-volatile and detection method technology, which is applied in the detection of 103 kinds of semi-volatile organic compounds and the detection of semi-volatile organic compounds in blood, can solve the problems of large manpower consumption of reagents, complicated processing process and long analysis time, etc. Achieve cost-effectiveness, high analytical efficiency, and reduced impurities and matrix interferences

Inactive Publication Date: 2021-02-19
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pretreatment process is complex, the reagents consume a lot of manpower, the requirements for instruments are large, and the analysis time is long

Method used

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  • Method for detecting semi-volatile organic compounds in blood
  • Method for detecting semi-volatile organic compounds in blood
  • Method for detecting semi-volatile organic compounds in blood

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] (1) Preparation of standard solution of semi-volatile organic compounds to be measured

[0067] Take an appropriate amount of each high-concentration single standard solution, and use n-hexane to prepare a single standard solution with a concentration of 10 μg / mL (7 items of phthalates, 7 items of polychlorinated biphenyls, 16 items of polycyclic aromatic hydrocarbons, polybrominated diphenyl 5 ethers), and methanol was used to prepare a single standard solution with a concentration of 10 μg / mL (68 pesticides).

[0068] (2) Optimization of chromatography / mass spectrometry conditions

[0069] Taking the use of chromatographic column DB-5MS (30*m*0.25mm*0.25μm) as an example, each 10μg / mL single standard solution is directly injected, and the full scan is performed first to find the molecular ion peak with high response and strong specificity. Parent ions (that is, molecular ions), and then set different collision energies according to pre-selected different collision en...

Embodiment 2

[0094] According to the triple quadrupole gas chromatography-mass spectrometry detection details parameter conditions set in Example 1, the whole blood of the volunteers was collected and centrifuged to obtain the serum; the serum was divided into 7 equal parts as parallel samples for the experiment. Specific steps are as follows:

[0095] (1) Multi-stage liquid-liquid extraction:

[0096] Add 0.1mL of the serum sample to be tested, add ultrapure water to dilute 2 times, add 0.5mL acetonitrile, seal the ultrasound for 5 minutes, add 1mL n-hexane, vibrate and extract for 5 minutes, take the supernatant after centrifugation, and record it as the first sample. supernatant;

[0097] Next, add 0.1 mL of dichloromethane to the above-mentioned treated serum sample again, vibrate and extract for 5 minutes, take the supernatant after centrifugation, and record it as the second supernatant;

[0098] The first supernatant and the second supernatant were combined, dried with pure nitrog...

Embodiment 3

[0116] According to the triple quadrupole gas chromatography-mass spectrometry detection details parameter condition setting determined in Example 1, another volunteer’s whole blood was collected, and the serum was obtained after centrifugation; the serum was divided into 7 equal parts as parallel samples, and the experiment was carried out . Specific steps are as follows:

[0117] (1) Multi-stage liquid-liquid extraction:

[0118] Dilute 2mL of the serum sample to be tested by adding ultrapure water to 3 times, add 2mL of acetonitrile, seal the ultrasound for 20 minutes, add 5mL of n-hexane, vibrate and extract for 5 minutes, take the supernatant after centrifugation, and record it as the first supernatant liquid;

[0119] Next, add 1mL of dichloromethane again to the above-mentioned treated serum sample, vibrate and extract for 5 minutes, take the supernatant after centrifugation, and record it as the second supernatant;

[0120] The first supernatant and the second super...

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Abstract

The invention belongs to the field of monitoring of organic pollutants in complex matrix biological samples, and discloses a method for detecting semi-volatile organic compounds in blood, which comprises the following steps of carrying out multistage extraction, then carrying out solid-phase purification, carrying out analysis by using a gas chromatograph-mass spectrometer, and finally, calculating the concentration of the semi-volatile organic compounds of each to-be-detected target. By improving the overall process flow design of the method, a sample to be detected is firstly subjected to specific pretreatment, and then the pretreated sample is detected by adopting a gas chromatograph-mass spectrometer multi-reaction monitoring mode; and a plurality of representative semi-volatile organic compounds such as phthalate, polycyclic aromatic hydrocarbon, polybrominated diphenyl ether, polychlorinated biphenyl, pesticide and the like in the blood are detected. The detection method has theadvantages of low detection limit, good recovery rate, high analysis efficiency and the like.

Description

technical field [0001] The invention belongs to the field of monitoring organic pollutants in complex matrix biological samples, and more specifically relates to a method for detecting semi-volatile organic compounds in blood, which is applicable to the detection of 103 semi-volatile organic compounds. Background technique [0002] Semi-volatile organic compounds are a class of boiling point between 170-350 ℃, vapor pressure at 1.3*10 -2 ~10 -8 Organic matter between KPa, including pesticides, polycyclic aromatic hydrocarbons, phthalates, flame retardants, polychlorinated biphenyls and polybrominated biphenyls and other compounds (Environ Res. 2017; 158:649-659). Semi-volatile organic compounds are widely found in plastic products, decoration materials and household daily chemicals. Human activities are the main source of semi-volatile organic compounds in the environment. With their unique physical characteristics, semi-volatile organic compounds can dissociate from the s...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/86
CPCG01N30/02G01N30/06G01N30/08G01N30/8679G01N2030/062
Inventor 荆涛汪秀黄凯
Owner HUAZHONG UNIV OF SCI & TECH
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