Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry

A technology of dimethyl sulfate and pyraclostrobin, which is applied in the field of analysis and can solve the problems of unchecked analysis and detection of dimethyl sulfate

Pending Publication Date: 2021-05-28
SUZHOU GUOCHEN BIOTEK CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Dimethyl sulfate is a necessary raw material in the synthesis route of pyraclostrobin technical drug, and there is no refer

Method used

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  • Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry
  • Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry
  • Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1, standard solution preparation

[0035] Weigh about 0.020g (accurate to 0.02mg) dimethyl sulfate standard sample, put it in a 50mL volumetric flask, dissolve it with dichloromethane, dilute to volume, and shake well. Accurately draw 5.00mL of the solution, and put it in a 100mL volumetric flask , dilute to volume with dichloromethane and shake well. Then accurately draw 5.00 mL of the standard stock solution, place it in a 250 mL volumetric flask, dilute to volume with dichloromethane, shake well, and prepare the standard parent drug with a mass concentration of 0.4 μg / mL.

Embodiment 2

[0036] Embodiment 2, standard curve:

[0037] Accurately pipette 4.00, 6.00, 10.00, 12.00, 15.00 and 20.00mL of 0.4μg / mL standard parent drug to prepare a standard working curve solution, and use the method of gas chromatography to draw the standard with the mass concentration as the abscissa and the peak area as the ordinate. curve to get the linear regression equation.

[0038] y=19284067.2149x-28.6500, R 2 = 0.9999.

Embodiment 3

[0039] The mensuration of dimethyl sulfate content in embodiment 3, sample

[0040] Weigh about 1.5g of the sample (accurate to 0.2mg), put it in a 25mL volumetric flask, add dichloromethane to dissolve, make up to volume, and shake well.

[0041] Using GC method, record the peak area of ​​dimethyl sulfate in the sample, and substitute the peak area into the standard curve linear regression equation to calculate the content of dimethyl sulfate.

[0042] Adopt gas chromatography-mass spectrometry (quadrupole mass analyzer) analysis condition is as follows:

[0043] Chromatographic column: HP-5MS cross-linked capillary column, 30m×0.25mm(i.d.)×0.25μm

[0044] Column temperature:

[0045] Carrier gas (He): 1.2mL / min;

[0046] Vaporization temperature: 250°C;

[0047] Ion source: EI, 70eV;

[0048] Ion source temperature: 230°C;

[0049] Quadrupole mass analyzer temperature: 150°C;

[0050] Split ratio: 10:1;

[0051] Detection mode: single ion scan m / z 95;

[0052] Inj...

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PUM

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Abstract

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to an analysis method for determining dimethyl sulfate in pyraclostrobin by a gas chromatography-mass spectrometry method. The invention discloses an analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry. The analysis method comprises the following steps: (1) preparing a standard solution; (2) drawing a standard curve; and (3) determining the content of dimethyl sulfate in the sample. Compared with the prior art, the method disclosed by the invention has the advantages of simplicity and convenience in sample preparation, small sample dosage and suitability for conventional determination; the sensitivity is high, and the lowest detection limit of dimethyl sulfate is 0.20 mg/kg. The method is simple in test process, high in sensitivity and good in accuracy.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to an analysis method for determining dimethyl sulfate in pyraclostrobin by gas chromatography-mass chromatography. Background technique [0002] Dimethyl sulfate is highly toxic, its effect is similar to that of mustard gas, and its acute toxicity is similar to that of phosgene, which is 15 times greater than that of chlorine gas. It has a strong irritating effect on eyes and upper respiratory tract and a strong corrosive effect on skin. It can cause conjunctival hyperemia, edema, corneal epithelial shedding, partial necrosis of tracheal and bronchial epithelial cells, and perforation leading to mediastinal or subcutaneous emphysema. In addition, it can also damage the liver, kidney and heart muscle, etc., and can cause burns, blisters and deep necrosis after skin contact. [0003] Dimethyl sulfate is a necessary raw material in the synthetic route of pyraclostrobin ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 孙剑英段鹏强刘天顺付大庆张瑞杰
Owner SUZHOU GUOCHEN BIOTEK CO LTD
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