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Method for reducing p, p'-DDT degradation rate in organochlorine pesticide analysis process

An analytical process and organochlorine technology, applied in the field of chromatographic analysis, can solve the problems of difficult to guarantee the accuracy of sample analysis, high cost of consumables, time-consuming and laborious maintenance, etc. Effect

Active Publication Date: 2020-03-31
四川省生态环境监测总站
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to provide a method for reducing the degradation rate of p,p'-DDT in the analysis process of organochlorine pesticides, which solves the problems of high cost of consumables, time-consuming and laborious maintenance, and Difficult to guarantee the accuracy of sample analysis

Method used

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  • Method for reducing p, p'-DDT degradation rate in organochlorine pesticide analysis process
  • Method for reducing p, p'-DDT degradation rate in organochlorine pesticide analysis process
  • Method for reducing p, p'-DDT degradation rate in organochlorine pesticide analysis process

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Experimental program
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Effect test

Embodiment 1

[0026] Prepare a p,p'-DDT standard solution with a n-hexane phase concentration of 20 μg / mL, inject and analyze separately to obtain the degradation rate of p,p'-DDT without adding degradation inhibitors, and then add 1.0 μL of chloroform ( Chemical formula CHCl 3 ), and the p,p'-DDT in the n-hexane phase was injected simultaneously to obtain the effect of chloroform on the degradation rate of p,p'-DDT, where the chromatographic split ratio was 2:1.

[0027] The gas chromatography mass spectrometry analysis conditions are as follows:

[0028] Inlet temperature: 270°C, split flow, split ratio: 2:1;

[0029] Injection volume of n-hexane phase p,p’-DDT: 1 μL

[0030] Chloroform injection volume: 1.0μL

[0031] Column flow: 1.0mL / min

[0032] Temperature program: 60°C for 2 minutes, 30°C / min to 225°C, hold for 0min, 1°C / min to 232°C, hold for 0min, 30°C / min to 300°C, hold for 1min

[0033] Gas interface temperature: 280°C

[0034] Mass spectrometry scanning method: SCAN, scann...

Embodiment 2

[0041] Prepare a p,p'-DDT standard solution with a n-hexane phase concentration of 20 μg / mL, inject and analyze separately to obtain the degradation rate of p,p'-DDT without adding degradation inhibitors, then add 1.0 μL chloroform, and The p,p'-DDT in the n-hexane phase was injected simultaneously to obtain the effect of chloroform on the degradation rate of p,p'-DDT, where the chromatographic split ratio was 20:1.

[0042] The gas chromatography mass spectrometry analysis conditions are as follows:

[0043] Inlet temperature: 270°C, split flow, split ratio: 20:1;

[0044] Injection volume of n-hexane phase p,p’-DDT: 1 μL

[0045] Chloroform injection volume: 1.0μL

[0046] Column flow: 1.0mL / min

[0047] Temperature program: 60°C for 2 minutes, 30°C / min to 225°C, hold for 0min, 1°C / min to 232°C, hold for 0min, 30°C / min to 300°C, hold for 1min

[0048] Gas interface temperature: 280°C

[0049] Mass spectrometry scanning method: SCAN, scanning range: 45 to 500 mass number...

Embodiment 3

[0056] Prepare calibration curves for 8 organochlorine pesticides, the 8 organochlorine pesticides are α666, β666, γ666, δ666, p,p'-DDE, p,p'-DDD, o,p'-DDT, p,p' -DDT, the concentration points of the calibration curve are 20μg / L, 50μg / L, 100μg / L, 200μg / L, 500μg / L, 1000μg / L, 2000μg / L, the internal standard is phenanthrene-d10, and the concentration is 500μg / L , 1 μL of chloroform was added to each injection to examine whether chloroform had any effect on the linearity of the calibration curve. The gas chromatography mass spectrometry analysis conditions are as follows:

[0057] Inlet temperature: 270°C, split ratio: 20:1;

[0058] Calibration curve injection volume: 1μL

[0059] Chloroform injection volume: 0.5μL

[0060] Column flow: 1.0mL / min

[0061] Temperature program: 60°C for 2 minutes, 30°C / min to 225°C, hold for 0min, 1°C / min to 232°C, hold for 0min, 30°C / min to 300°C, hold for 1min

[0062] Gas interface temperature: 280°C

[0063] Mass spectrometry scanning met...

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Abstract

The invention discloses a method for reducing p, p'-DDT degradation rate in organochlorine pesticide analysis process, and solves the problems of high consumable cost, time and labor waste in maintenance and difficulty in guaranteeing the sample analysis accuracy in a current treatment method for p, p'-DDT degradation problems. The method disclosed by the invention comprises the following steps: sampling a sample extracting solution containing the organochlorine pesticide through a liquid sample injector, introducing the sample extracting solution into a chromatographic system, and adding 0.1-1.0 mu L of a degradation inhibitor at the same time, so as to inhibit p, p '-DDT degradation; the degradation inhibitor is an organic compound with a halogen group strong electronegative group, and the general formula of the degradation inhibitor is any one of CnH2n-xClx, CnH2n + 2-xClx and CnH2n + 2-xIx. By means of the scheme, the degradation rate of p, p '-DDT can be kept below 15% in the organochlorine pesticide analysis process, the analysis stability is guaranteed, the analysis accuracy is greatly improved, the maintenance frequency of a chromatographic system is reduced, and the analysis cost and the analysis time are effectively saved. Therefore, the method is very suitable for large-scale popularization and application.

Description

technical field [0001] The invention relates to the technical field of chromatographic analysis, in particular to a method for reducing the degradation rate of p,p'-DDT during the analysis of organochlorine pesticides. Background technique [0002] At present, during the analysis of organochlorine pesticides by gas chromatography or gas chromatography / mass spectrometry, p,p’-DDT is easily degraded during the analysis process, resulting in sample analysis failure. The reason for the degradation of p,p'-DDT is that when the injection port and chromatographic system are not clean and there are more active sites, these The active sites produced catalyst-like properties that degraded p,p'-DDT into p,p'-DDE and p,p'-DDD. According to the provisions of "HJ921-2017 Determination of Organochlorine Pesticides in Soil and Sediment by Gas Chromatography", the degradation rate of p,p'-DDT%=peak area (P,P'-DDE+P,P'-DDD) / Peak area (P, P'-DDE+P, P'-DDD+P, P'-DDT), when the degradation ra...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/16
CPCG01N30/06G01N30/16
Inventor 张渝程小艳
Owner 四川省生态环境监测总站