Gas chromatography-mass spectrometry detection method for hexachlorobenzene and decabromodiphenyl in chlorothalonil

A decachlorobiphenyl and gas chromatography technology, which is applied in the field of gas chromatography-mass spectrometry detection of hexachlorobenzene and decachlorobiphenyl in chlorothalonil, can solve the problem of decreased sensitivity and repeatability, impact on analysis efficiency, high maintenance cost, etc. problems, to achieve the effect of improving continuity and stability, improving detection efficiency, and shortening detection time

Pending Publication Date: 2022-02-01
JIANGSU XINHE AGROCHEM
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Problems solved by technology

Among the various detection methods described, the detection sensitivity of liquid chromatography cannot meet the requirements of ultra-trace determination. Although the FAO gas chromatography-mass spectrometry has higher sensitivity and selectivity, it can be because the trace amount in chlorothalonil is measured. Impurities, in order to improve the sensitivity, a large amount of chlorothalonil sample matrix is ​​introduced into the mass spectrometer detector in the method. On the one hand, it is easy to cause rapid contamination of the ion source in a short time, and the sensitivity and repeatability drop rapidly. Frequent cleaning will cause high maintenance costs and affect the analysis efficiency. On the other hand, in order to reduce the influence of the solvent effect of splitless injection, a lower initial temperature is adopted in the method, and the analysis time is longer.
[0006] In the current research method, gas chromatography-mass spectrometry is used to measure the impurities hexachlorobenzene and decachlorobiphenyl in chlorothalonil, but the operating conditions of chromatography and mass spectrometry are not ideal, and the sensitivity is low. The detection of chlorinated biphenyls, and the impact of ion source pollution on the detection also exists
[0007] Therefore, these current methods are difficult to meet the high sensitivity, repeatability, accuracy and rapid detection requirements of ultra-trace hexachlorobenzene and decachlorobiphenyl in batch chlorothalonil products of production enterprises

Method used

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  • Gas chromatography-mass spectrometry detection method for hexachlorobenzene and decabromodiphenyl in chlorothalonil
  • Gas chromatography-mass spectrometry detection method for hexachlorobenzene and decabromodiphenyl in chlorothalonil
  • Gas chromatography-mass spectrometry detection method for hexachlorobenzene and decabromodiphenyl in chlorothalonil

Examples

Experimental program
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preparation example Construction

[0105] (5) Preparation of chlorothalonil sample solution:

[0106] Weigh 0.2g (accurate to 0.0001g) of chlorothalonil sample, put it in a stoppered glass bottle, add 10mL xylene with a pipette, shake it in ultrasonic wave for 10min to dissolve it, cool to 25°C, shake well , to obtain chlorothalonil sample solution.

[0107] (6) 2μg / mL hexachlorobenzene-decachlorobiphenyl standard sample total ion chromatogram scan

[0108] Hexachlorobenzene-decachlorobiphenyl standard sample total ion chromatogram (TIC) scans, and the sample that described total ion chromatogram detects is the hexachlorobenzene-decachlorobiphenyl solution of 2 μ g / mL, and concrete steps are to comprise:

[0109] Use a pipette to take 2 mL each of the hexachlorobenzene single-standard stock solution and the decachlorobiphenyl single-standard stock solution in a 100 mL volumetric flask, dilute to the mark with xylene, shake well, and prepare the 2 μg / mL of hexachlorobenzene-decachlorobiphenyl standard solutio...

Embodiment 1

[0115] This example provides a gas chromatography-mass spectrometry detection method for hexachlorobenzene and decachlorobiphenyl in chlorothalonil.

[0116] Set the instrument conditions, gas chromatography conditions: where the temperature of the chromatographic column is programmed temperature rise, the initial column temperature is 140°C, the initial column temperature is maintained for 1.0min, and the temperature is raised to the first-order end point temperature of 240°C at a first-order heating rate of 40°C / min, and then Rise to the final column temperature of 320 °C at a second-stage temperature increase rate of 20 °C / min, and hold the final column temperature for 2 min; the carrier gas is helium, with a purity of ≥99.999%, and a flow rate of 1.0 mL / min. The temperature of the injection port was 280°C; the injection volume was 1.0 μL; the injection method was split injection, and the split ratio was 5:1.

[0117] Mass spectrometry detection conditions: ionization mode ...

Embodiment 2

[0133] This example provides a gas chromatography-mass spectrometry detection method for hexachlorobenzene and decachlorobiphenyl in chlorothalonil.

[0134] The only difference from Example 1 is that in the method described in this example, the initial temperature is 135° C. and kept for 0.5 min, and the temperature is raised to the first-order end point temperature of 245° C. at a first-order heating rate of 45° C. / min; the closing time of the mass spectrometer detector is 0.25min after the hexachlorobenzene retention time, all the other conditions are consistent with Example 1.

[0135] The specific gas chromatography conditions are as follows: the temperature of the chromatographic column is programmed temperature rise, the initial column temperature is 135°C, the initial column temperature is maintained for 0.5min, and the temperature is raised to the first-order end point temperature of 245°C at a first-order heating rate of 45°C / min, and then The second-stage temperatur...

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Abstract

The invention provides a gas chromatography-mass spectrometry detection method for hexachlorobenzene and decabromodiphenyl in chlorothalonil. The gas chromatography-mass spectrometry detection method comprises the following steps: preparing a hexachlorobenzene-decabromodiphenyl standard working solution and a chlorothalonil sample solution; separating and detecting the hexachlorobenzene-decabromodiphenyl standard working solution and the chlorothalonil sample solution by using gas chromatography and mass spectrometry, wherein the gas chromatography adopts a DB-5ms capillary column and is carried out in a split-flow sample injection manner; and obtaining a hexachlorobenzene standard curve and a decabromodiphenyl standard curve according to detection results of the gas chromatography and the mass spectrometry, and obtaining the content of the ultra-trace hexachlorobenzene and the decabromodiphenyl in the chlorothalonil sample solution by combining the standard curves. The gas chromatography-mass spectrometry detection method can sensitively and rapidly measure the content of ultra-trace hexachlorobenzene and decabromodiphenyl in high-purity chlorothalonil at the same time, the analysis cost is reduced, the analysis efficiency is high, and the gas chromatography-mass spectrometry detection method is suitable for measuring the content of ultra-trace hexachlorobenzene and decabromodiphenyl in a large batch of chlorothalonil products.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a gas chromatography-mass spectrometry detection method for hexachlorobenzene and decachlorobiphenyl in chlorothalonil. Background technique [0002] Chlorothalonil is a high-efficiency, low-toxicity, broad-spectrum, low-residue protective fungicide, which is widely used in the control of fungal diseases in agriculture and forestry. Hexachlorobenzene and decachlorobiphenyl are by-product impurities formed in the production process of chlorothalonil, which are persistent organic pollutants that are difficult to degrade, easy to accumulate in organisms and the environment, and are harmful to human body. Hazardous substances capable of causing cancer. [0003] The national standards for chlorothalonil and the FAO standards of the International Food and Agriculture Organization list it as a key control item and put forward strict requirements: the content of hexachlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/72G01N30/8679
Inventor 王振宇沙海洋王佩刘庆王晴
Owner JIANGSU XINHE AGROCHEM
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