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A method and device for simultaneously detecting three metabolites of chlorpyrifos in urine

A technology for metabolites and chlorpyrifos is applied in the field of simultaneous detection of three metabolites of chlorpyrifos in urine, which can solve the problems of inability to accurately qualitative and quantitative, false positive results, and inability to analyze and monitor requirements for metabolites of chlorpyrifos, and achieve accurate and reliable qualitative results. High accuracy and the effect of improving qualitative accuracy

Active Publication Date: 2019-10-25
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] And the gas chromatography-flame ionization detector, gas chromatography-electron capture detector, gas chromatography-nitrogen and phosphorus detector, high performance liquid chromatography-ultraviolet detector, etc. used in the previous methods are very useful for the simultaneous detection of three kinds of chlorpyrifos metabolites. On the one hand, in the face of complex background and many interfering substances, accurate qualitative and quantitative results cannot be obtained, and even false positive results appear, which is far from meeting the requirements for the analysis and monitoring of trace chlorpyrifos metabolites in human samples (such as urine and plasma).

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  • A method and device for simultaneously detecting three metabolites of chlorpyrifos in urine
  • A method and device for simultaneously detecting three metabolites of chlorpyrifos in urine
  • A method and device for simultaneously detecting three metabolites of chlorpyrifos in urine

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Experimental program
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Effect test

Embodiment 1

[0040] (1) Standard curve preparation:

[0041] Accurately weigh 0.01±0.0001 g of chlorpyrifos metabolite standard sample and internal standard (DBP) (Dr. Ehrenstorfer GmbH, Germany) into a 10 mL volumetric flask, dissolve with acetonitrile and constant volume to obtain TCPyr, DEP, DETP and internal standard DBP standard stock solution. And dilute with acetonitrile to prepare working solutions with concentrations of 0.005, 0.01, 0.02, 0.05, 0.10, 0.20 mg / L.

[0042] (2) Instrument analysis conditions:

[0043] Instrument chromatographic conditions: the ultra-high performance liquid chromatography is 1290Infinity of Agilent Company; the chromatographic column selects Agilent reversed-phase C18 chromatographic column (ZORBAX Eclipse Plus C18 3.5 μ m, 2.1 × 150mm, Agilent), column temperature is 35 ℃, mobile phase A 0.2‰ ammonia water, the mobile phase B is acetonitrile, the flow rate is 0.3mL / min, the injection volume is 2μL; the mobile phase gradient is:

[0044] ti...

Embodiment 2

[0052] A method for simultaneously detecting three metabolites of chlorpyrifos in urine, comprising the following steps:

[0053] (A) Three metabolites of chlorpyrifos were selected as the target compound: 3,5,6-trichloro-2-pyridinol, diethyl phosphate, and diethyl phosphorothioate;

[0054] (B) Weigh 6 blank urine samples, 10.0mL (±0.01mL) for each urine sample, divide them into two groups on average, add 0.01mg / kg, 0.050mg / kg, 0.20mg / L standard solution of chlorpyrifos metabolites respectively According to the above-mentioned sample pretreatment method: add 4mL HCl (6M) for shaking, and hydrolyze for 2h in a water bath at 80°C. After 2h, it was taken out and cooled to room temperature.

[0055] (C) Extraction: Add 10 mL of acetonitrile solution and 3 g of NaCl to the urine sample, vortex and mix for 1 min, then centrifuge at 8000 r / min, and take the upper layer of 5 mL of acetonitrile;

[0056] (D) Purification and concentration: Pass the extracted acetonitrile through a s...

Embodiment 3

[0064] (A) The target compound is 3,5,6-trichloro-2-pyridinol, diethyl phosphate and diethyl phosphorothioate;

[0065] (B) Sample collection: The sampling time was September 2, 2016, and the sampling location was Yaxi Town, Gaochun District, Nanjing City, and the tested urine samples were from children;

[0066] (C) Enzymatic hydrolysis: take frozen urine sample and thaw slowly at room temperature, take 10 mL of urine sample into a 50 mL centrifuge tube, add 4 mL of HCl (6M) for shaking, hydrolyze in 80 °C water bath for 2 hours, take it out after 2 hours, and cool down to room temperature;

[0067] (D) Extraction: Add 10 mL of acetonitrile solution and 3 g of NaCl to the urine sample, vortex and mix for 1 min, and after centrifugation, take the upper layer of 5 mL of acetonitrile;

[0068](E) Purification and concentration: pass the extracted acetonitrile through a self-made purification column, and then elute with 5mL acetonitrile after loading the sample, collect all the e...

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Abstract

The invention discloses a method and a device for simultaneously detecting three metabolic products of chlorpyrifos in urine. The method comprises the following steps: (A) target compounds selection: selecting 3,5,6-trichloro-2-pyridoxol, triethyl phosphate and diethyl thiophosphate; (B) sample enzymolysis; (C) sample extraction; (D) sample purification and concentration; (E) instrumental analysis. The device mainly comprises a main body and a chromatography-ion tandem mass spectrum detector, wherein the main body comprises a power supply unit, a thawing unit, a centrifugal device I, a water bath device, a turbine mixing device, a centrifugal device II, a purification device, a rotary evaporation device and a PLC (programmable logic controller). According to the method disclosed by the invention, the detection effectiveness and the detection reliability are greatly improved, and the detection time and the detection cost are saved.

Description

technical field [0001] The invention relates to the technical field of pesticide detection, in particular to a method and a device for simultaneously detecting three metabolites of chlorpyrifos in urine. Background technique [0002] Chlorpyrifos belongs to a broad-spectrum organophosphorus insecticide widely used in the control of various diseases and insect pests of crops. Chlorpyrifos is the leading pesticide variety in my country's insecticide market, and its production and usage in the world are also high. Chlorpyrifos can enter the human body through exposure to food, air, soil and other media. [0003] Chlorpyrifos can inhibit the activity of choline ester, and the acetylcholinesterase in the central nervous system plays an important role in maintaining the occurrence and maturation of nerve cells in the central nervous system. More and more studies have confirmed that chlorpyrifos has chronic toxic effects on the developing central nervous system, which is related ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08
CPCG01N30/02G01N30/06G01N30/08
Inventor 徐怀洲吉贵祥张圣虎张芹韩志华宋宁慧吴晟旻刘济宁石利利
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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