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Method for extracting toxaphene pesticide residue in tobacco and tobacco products

A technology for tobacco products and pesticide residues, which is applied in the field of analysis and detection of tobacco pesticide residues, can solve the problems of organic solvent exposure, cumbersome operation, and long time consumption, and achieve the effects of fast extraction speed, improved extraction efficiency, and easy operation

Inactive Publication Date: 2012-10-17
CHINA TOBACCO GUANGXI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The industry standard YC / T 180-2004 for the detection of toxaphene in tobacco is also determined by this method. The pre-treatment method is the Soxhlet extraction method, which has high accuracy, but the operation is cumbersome and time-consuming. It takes 5-6 hours to process a sample. , and the testers are more exposed to organic solvents

Method used

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  • Method for extracting toxaphene pesticide residue in tobacco and tobacco products
  • Method for extracting toxaphene pesticide residue in tobacco and tobacco products
  • Method for extracting toxaphene pesticide residue in tobacco and tobacco products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Pretreatment of florisil is carried out by placing the florisil in a quartz crucible, burning it in a muffle furnace at 550°C for at least 5 hours, cooling it in a desiccator without a desiccant, and then transferring it to In a round bottom flask, add 5ml of water per 100g, mix thoroughly in a rotary flask for about 1h, and balance in a closed glass container for at least 48h.

[0019] Put the tobacco leaves in an oven, keep at 50°C for 2 hours, grind the samples, pass through a 2mm (10 mesh) sieve, pay attention that the grinding temperature does not exceed 50°C, and measure the moisture content according to YC / T 31, and the obtained samples are ready for accelerated solvent extraction.

[0020] Put a layer of fiber filter paper at the bottom of the 33ml stainless steel extraction tank, then weigh 5g±0.05g of pretreated florisil and transfer it to the extraction tank, then accurately weigh 5g of smoke powder (accurate to 0.01g) and 5g±0.05 g pretreated florisil, groun...

Embodiment 2

[0029] Take a certain amount of tobacco stems and utilize the accelerated solvent extraction method to extract toxaphene according to the method of embodiment 1 and detect, and the results of calculating the relative standard deviation and recovery of toxaphene are shown in Table 2.

[0030] Table 2 precision and recovery experiment (n=6)

[0031]

Embodiment 3

[0033] Take a certain amount of tobacco flakes and utilize the accelerated solvent extraction method to extract toxaphene according to the method of embodiment 1 and detect, and the results of calculating the relative standard deviation and recovery rate of toxaphene are shown in Table 3.

[0034] Table 3 precision and recovery experiment (n=6)

[0035] .

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Abstract

The invention discloses a method for extracting toxaphene pesticide residue in tobacco and tobacco products. The method comprises the steps of preprocessing tobaccos and tobacco products, weighing processed tobaccos or tobacco products and preprocessed cleanert florisil, grinding uniformly and then transferring to a stainless steel extraction pool, and operating an accelerated solvent extractor to extract toxaphene. The parameters of the accelerated solvent extractor are as follows: the temperature is 100 DEG C, the pressure is 1500psi, the heating time is 5 minutes, the standing time is 5 minutes, the washing volume is 60%, the nitrogen purging time is 60 seconds, and the static cycle time is 2. The used solvent is acetone and normal hexane, wherein the volume ratio of the acetone to the normal hexane is 1:1. An HP-5 chromatographic column is taken as an analytical column, and the toxaphene content in the tobacco or the tobacco products is determined by gas chromatography equipped with an electron capture detector. The method has the characteristics that the operation is simple and convenient, the analysis speed is quick, the sensitivity is high, and the accuracy and the stability are good, and is particularly suitable for analysis of the toxaphene pesticide residue in mass tobaccos and the tobacco products.

Description

technical field [0001] The invention relates to the technical field of analysis and detection of tobacco pesticide residues, in particular to a method for extracting tobacco toxaphene pesticide residues. The method utilizes an accelerated solvent extraction apparatus to extract tobacco toxaphene. Background technique [0002] Toxaphene is a broad-spectrum organochlorine insecticide, composed of 175-179 polychlorinated alkanes and polychlorinated camphenes, and is one of the 12 priority persistent organic pollutants. Since the 1940s and 1950s, toxaphene has been widely produced and used as a substitute for DDT and cyclopentadiene pesticides around the world, causing great harm to the ecological environment and human health. Therefore, it is very important to establish a rapid, sensitive and accurate analytical method to analyze and detect toxaphene residues in tobacco. [0003] Currently, Soxhlet extraction and gas chromatography-electron capture detector (GC-ECD) are common...

Claims

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Application Information

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IPC IPC(8): G01N30/06
Inventor 周晓黄泰松李小兰陈志燕冯守爱周芸王维刚胡斌
Owner CHINA TOBACCO GUANGXI IND