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Method for determining content of paraquat in blood with gas chromatography-mass spectrometry

A technology of gas chromatography and mass spectrometry, applied in the field of paraquat content, can solve the problems of applicability and insufficient accuracy

Inactive Publication Date: 2017-04-26
NANJING YITE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main methods for the determination of paraquat are spectrophotometry and high performance liquid chromatography, but their applicability and accuracy are slightly insufficient

Method used

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  • Method for determining content of paraquat in blood with gas chromatography-mass spectrometry
  • Method for determining content of paraquat in blood with gas chromatography-mass spectrometry
  • Method for determining content of paraquat in blood with gas chromatography-mass spectrometry

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Experimental program
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Embodiment Construction

[0012] The technical solution of the present invention will be described in detail below in conjunction with specific implementation.

[0013] Method for the determination of paraquat content in blood by gas chromatography-mass spectrometry:

[0014] 1. Instrument:

[0015] Agilent GC / MS 5975B (with autosampler, Agilent, USA)

[0016] Desktop high-speed refrigerated centrifuge (CT15RT, Shanghai Tianmei Company)

[0017] High-speed dispersing homogenizer (Germany IKA company)

[0018] Nitrogen blower

[0019] ultrasonic cleaner

[0020] Vortex mixer

[0021] Various glassware, etc.

[0022] 2. Reagents:

[0023] Paraquat (dichloride salt, purity ≥98.8%)

[0024] Acetonitrile (chromatographically pure)

[0025] Methanol (chromatographically pure)

[0026] Ultra-pure water.

[0027] 3. Analysis and determination:

[0028] Sample pretreatment

[0029] Take 1 mL of whole blood and add dropwise into a 15 mL centrifuge tube containing 4 mL of acetonitrile and 50 μL of fo...

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Abstract

The invention discloses a method for determining the content of paraquat in blood with a gas chromatography-mass spectrometry. The method comprises a sample treatment step and an assay determination step, in the assay determination step, the gas phase condition of a gas chromatograph is set as follows: an HP-5MS (30 m*250 mu m, 0.25 mu m) capillary chromatographic column is adopted, the column box temperature is kept at 50 DEG C for 1 min, increased to 200 DEG C at 10 DEG C / min, increased to 250 DEG C at 40 DEG C / min and kept at 260 DEG C for 4 min; the interfere temperature of gas chromatography and mass spectrometry is 280 DEG C. The result detection data of the paraquat in blood are accurate, and the method meets the national requirement and is time-saving and efficient. A qualitative and quantitative method that anticoagulant of a patient is detected through mass spectrometry full scanning after simple pretreatment is established, and the method detection limit is 0.2 mg / L; the detection result of the same blood is relatively stable, and the relative standard deviation is smaller than or equal to 10%. In conclusion, the method is simple and quick to operate, the reagent cost is low, and the assay result is reliable.

Description

technical field [0001] The invention relates to a method for measuring paraquat content in blood by gas chromatography-mass spectrometry, and belongs to the field of clinical treatment. Background technique [0002] Paraquat (paraquat), aliased as Kewuzong, Paraquat, Wildfire, Baiduo, Baraquat, etc., chemical name 1,1-dimethyl-4,4-bipyridine cationic salt, is an organic heterocyclic herbicide agent. Among them, dichloride salt accounts for the majority. The pure product is a white crystal, easily soluble in water, slightly soluble in low molecular weight alcohols, stable in acidic and neutral solutions, and easily decomposed in alkaline solutions. Oral administration is the main route of poisoning, and the fatality rate of poisoning is extremely high. The absorption rate of paraquat in the gastrointestinal tract is 5% to 15%, and oral administration of 5 mL to 15 mL of commercially available 20% paraquat water is enough to cause death. At present, the main methods for th...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 洪霞张淑雅刘静
Owner NANJING YITE BIOTECH