KR101895342B1 - Method for Pre-treating a Sample Containing Dioxine and Furane Using Multi-Layer Silica Gel Column - Google Patents

Abstract

The present invention relates to a pretreatment method of a sample for analyzing dioxin or furan using a multi-layered silica gel column. More specifically, the present invention simplifies two steps of a sulfuric acid treatment process and a silica gel column purification process in a conventional pretreatment method of a sample for analyzing dioxin or furan to purify the sample with a multi-layered silica gel column, and reduces the pretreatment step and drastically reduces the time required by concentrating the purified sample under a proper temperature by heating in a nitrogen atmosphere. According to the present invention, compared to the conventional pretreatment method, the purification process and the concentration process can be shortened and the use of the analysis reagent can be reduced by simplifying the process.

Description

[TECHNICAL FIELD] The present invention relates to a method for pretreating a sample for analysis of dioxin or furane using a multi-layered silica gel column,

The present invention relates to a pretreatment method and an analytical method for a sample for analyzing dioxin or furan using a multi-layered silica gel column, and more particularly to a pretreatment method of a sample for analyzing a dioxin or furan analogue using a sulfuric acid treatment process and a silica gel column purification process , A pretreatment method of dioxins or furans, which reduces the time required for pretreatment by reducing the pretreatment stage by pretreatment with a multilayer silica gel column, and a pretreatment method of dioxins or furans such as dioxins or furans which perform a high-resolution gas chromatography or mass spectrometry And the like.

Endocrine disruptors, which have attracted much attention in the international community in recent years, are not only highly toxic but also are not well decomposed. They have the characteristics of internal accumulation of organisms, move through the air, water, and regenerative organisms, It is also pointed out that it can cause many problems in the ecosystem if it is released into the environment.

Dioxins, one of the typical endocrine disruptors, are unintentionally generated and discharged as a result of incomplete combustion or chemical reaction in a thermal process involving organic matter and chlorine. Dioxins are collectively referred to as polychlorinated dibenzodioxins (PCDD) and ploychlorinated dibenzofuranes (PCDF). These forms of dioxins are a form of mixed co-materials Present or exposed. Dioxins or furans may theoretically have 210 isomers depending on the number of chlorine atoms and the substituted position. In the present environment, about 130 species are detected.

According to the process test method of dioxins in domestic and US, the quantitative analysis of dioxins or furans is prescribed to be carried out in a high-resolution mass spectrometer because the amount of these substances present is very small, and dioxins or furans Because there are many interfering substances with very similar chemical and physical properties. A high-resolution mass spectrometer (resolution = 10,000 or more) and isotope dilution method are applied to minimize the influence of such interference substances.

The quantitative determination of 2,3,7,8-TCDD, which is the most toxic, is detected from the isotope of chlorine (Cl) substituted in the above compound by the molecular weight (M +) and in the portion having 2 higher molecular weight (M ++ 2) Is calculated as the sum of the peak widths. At this time, it is very important whether the peak ratio (M + / M ++ 2) in the dioxin analysis meets the theoretical value because the accuracy of this ratio means that there is no possibility of other interference substances. If this range is exceeded, it can be seen that the removal of the interfering substance is not perfect in the pre-treatment process, and the reliability of the quantification result is lowered. For example, in the case of 2,3,7,8-TCDD to be measured in the present invention, it is precisely in the range of 0.65 to 0.89.

In the case of other dioxins, it will appear at different retention values and other molecular weights. Usually, in order to obtain the results satisfying these peak ratios, analysis is carried out in the order of sampling → extraction → pre-treatment (interference substance removal process) → qualitative / quantitative analysis (high resolution gas chromatography or mass spectrometer) This method is adopted.

The most important process that determines the success or failure of dioxin or furan analysis is the pretreatment process, which is the process of removing interferences. Many kinds of substances are mixed in the concentrated liquid extracted from the sample collected in the environment. Among the dioxins and furans, there exist very small amounts of dioxins and furans at a level of ng (grams) to picogram (pg) , It is necessary to completely remove other substances and to concentrate only dioxins or furans in the pretreatment process. Pre-treatment of dioxins or furans designated by the US EPA or the Ministry of Environment is conducted through the following three steps of column chromatography (EPA1613 method).

(1 g) containing silica gel (1 g) / KOH (4 g, basic silica gel) / silica gel (1 g) in which the extract was extracted with toluene, (Diameter 1 cm, length 30 cm) filled with silica gel (8 g) / silica gel (2 g) / H ₂ O ₂ containing silica gel (2 g) and eluted with 100 ml of normal hexane.

Step 2 - Concentrate the n-hexane layer eluted in the above step 1 to about 1 ml, and then add 100 ml of normal hexane, 100 ml of dichloromethane: normal hexane (2:98) 100 ml of dichloromethane: normal hexane (50: 50), and finally 100 ml of eluted dichloromethane: n-hexane (50: 50) is concentrated to about 1 ml.

Step 3 - About 1 ml of concentrated dichloromethane: n-hexane (50:50) concentrated in the above step 2 was poured on the bottom, 9 g of trade name Carbopak C (manufactured by Supelco, serial number 1-0258) and trade name celite 545 (Manufactured by Supelco, USA, serial number 2-0199), the column was subjected to column chromatography according to the following procedure, and finally the eluted fractions were concentrated to a final concentration of 50 to 100 μl and quantitatively analyzed on a high resolution gas chromatography or mass spectrometer (1: 1, v / v) of a mixed solution of 5 ml of toluene / methylene chloride: methanol: toluene (15: 4: 1) / 2 ml of methylene chloride / cyclohexane v) 1 ml / hexane 5 ml. 2) Elimination of interfering substances = 2 ml of a mixed solution of 3 ml of hexane / 2 ml of methylene chloride / cyclohexane (1: 1, v / v) / methylene chloride: methanol: toluene (15: 4: 1) 3) Dioxin elution: Change the vertical position of the column and use 20 ml of toluene to separate dioxin or furans directly from the layer from which dioxin or furans have been extracted.

In the first step, the interference material having a large polarity is removed, and in the second step, the relatively non-polar interference material is removed. For example, in the second step, polyaromatic hydrocarbons (PAH) are removed using n-hexane and polychlorinated biphenyls (PCBs) are removed using dichloromethane: n-hexane (2:98) Finally, dichloromethane: n-hexane (50:50) is used to elute dioxins or furans.

However, since such a preprocessing method is described in a general and comprehensive manner, some problems may occur as follows.

First, the analysis of dioxins or furans differs depending on the type of impurities due to the analysis of trace amounts of micro-mass analysis, so the pretreatment method may vary depending on each medium. Second, the existing preprocessing method is complicated and takes a lot of time. Third, a large amount of reagent (solvent) is required in the pretreatment process, resulting in an increase in the cost of analyzing dioxins or furans.

Thus, the analysis of dioxins or furans is complicated and requires a lot of time and labor to produce analytical data based on relevant policies.

Therefore, it is possible to obtain data with a simple, fast and reliable accuracy by improving the preprocessing method which is complicated and consumes a lot of time and reagent, and can perform efficient work through cost reduction and provide high quality data, And to use it as basic data.

Japanese Laid-Open Patent Application No. 2006-0095504 discloses a method for detecting dioxins or furans using a chlorination reaction and a pretreatment method for analyzing dioxins or furans analytical samples using an activated copper powder, The accuracy of dioxin or furan analysis was improved. However, the method of detecting dioxins or furans using a chlorination reaction has a disadvantage in that the consumption time is prolonged in the purification process in the column as compared with the conventional method. In addition, the pretreatment method of the sample for analyzing dioxin or furan using the activated copper powder is not easy because the conditions for activating the copper powder and the storage condition of the activated copper powder are severely hampered, There is a disadvantage that there is a serious error in the error.

Japanese Patent Application Laid-Open No. 2006-0095504

The present invention has been developed to solve the above-mentioned problems. It is an object of the present invention to provide a method for removing dioxins or furans from an organic material, a coloring material and a polar material, The present invention provides a method for simplifying the step of using a multilayer silica gel column and heating the sample in a nitrogen atmosphere in concentration of the extracted sample through a purification process so as to shorten the pretreatment time of the entire analytical sample.

It is another object of the present invention to provide a method for analyzing dioxins or furans characterized by injecting a pretreated sample into high-resolution gas chromatography or mass spectrometry.

In order to solve the above-mentioned problems, the present invention provides a method for producing an extract, comprising: (a) preparing an extract for extracting dioxin or furans-containing extract from a sample using a solvent; (b) a first concentrate preparation step of removing the solvent from the extract; (c) a primary chromatographic step of fractionating said primary concentrate using a multi-layered silica gel column; (d) a second concentrate preparation step for concentrating the fraction after the first chromatography step; (e) a second chromatographic step of fractionating the second concentrate using a column packed with alumina; And (f) a step of obtaining a sample for analysis by concentrating the fraction subjected to the secondary chromatography step, to provide a method for pretreating a sample for dioxin or furan analysis.

In the pretreatment method of a sample for dioxin or furan analysis according to the present invention, the multilayer silica gel column is packed in the order of neutral silica gel, potassium hydroxide silica gel, sulfuric acid silica gel, neutral silica gel, silver silver nitrate silica gel, anhydrous sodium sulfate, .

In the pretreatment method of a sample for dioxin or furan analysis according to the present invention, the multi-layered silica gel column may be a neutral silica gel, potassium hydroxide silica gel, primary sulfuric acid silica gel, secondary sulfuric acid silica gel, neutral silica gel, silver nitrate silver sulfate, Particle layer, wherein the first sulfuric acid silica gel is 44% sulfuric acid silica gel and the second sulfuric acid silica gel is 22% sulfuric acid silica gel.

In the pretreatment method of a sample for dioxin or furan analysis according to the present invention, the first sulfuric acid silica gel has an average particle size of 100 to 150 탆, the second sulfuric acid silica gel has an average particle size of 30 to 50 탆, 1 to 1.5 times as much as the weight of the sulfuric acid silica gel.

In the pretreatment method of a sample for dioxin or furan analysis according to the present invention, the solvent may be toluene.

In the pretreatment method of a sample for dioxin or furan analysis according to the present invention, the sample may be concentrated by heating in a nitrogen atmosphere.

In addition, the present invention provides a method for analyzing dioxin or furan by injecting a sample pretreated by the pretreatment bamboo into a high-resolution gas chromatography or mass spectrometry.

Further, the present invention provides a multilayer silica gel column for dioxin or furan analysis, which is packed in the order of neutral silica gel, potassium hydroxide silica gel, sulfuric acid silica gel, neutral silica gel, silver silver nitrate silica gel, anhydrous sodium sulfate and copper particle layer.

As described above, the present invention simplifies the pretreatment process of the sample for analysis of dioxin or furan by pretreating the sample using the multilayer silica gel column, thereby reducing the processing time and dramatically reducing the analysis reagent.

FIG. 1 shows a conventional pretreatment method of a sample for analyzing dioxin or furan.
FIG. 2 shows a pretreatment method of a sample according to the present invention.
3 is a schematic view of a multilayer silica gel column according to the present invention.
FIG. 4 shows a conventional sulfuric acid treatment process, a silica gel column purification process, and a multi-layer silica gel column purification process according to the present invention.
FIG. 5 shows a conventional concentration process and a concentration process according to the present invention.
6 is a mass chromatogram of 2,3,7,8-TCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
7 is a mass chromatogram of 1,2,3,7,8-PeCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
8 is a mass chromatogram of 2,3,4,7,8-PeCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
9 is a mass chromatogram of -hXCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
10 is a mass chromatogram obtained when -hXCDF is analyzed in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
11 is a mass chromatogram of -HpCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
12 is a mass chromatogram of OCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
13 is a mass chromatogram of 2,3,7,8-TCDD in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
14 is a mass chromatogram of -HxCDD in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
15 is a mass chromatogram of 1,2,3,4,6,7,8-HpCDF in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
16 is a mass chromatogram of OCDD in a sample for analysis of dioxin or furan by the pretreatment method of the present invention.
FIG. 17 is a mass chromatogram obtained when the internal standard substance for sample extraction, 37Cl4-2,3,7,8-TCDD, was analyzed by the pretreatment method of the present invention.

Hereinafter, the present invention will be described in detail. The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms and the inventor may appropriately define the concept of the term in order to best describe its invention It should be construed as meaning and concept consistent with the technical idea of the present invention.

The term " dioxin or furan " as used throughout the specification of the present invention means a compound having 2, 3, 7, 8, or 8, which has a structure in which chlorine atoms are substituted at positions 2, 3, 7, - tetrachlorinated dibenzo-ρ-diozine (hereinafter referred to as 2,3,7,8-TCDD) is a representative compound, and polychlorinated dibenzo-dioxin dibenzodioxins (PCDD) and ploychlorinated dibenzofuranes (PCDF). These two substances are present or exposed in the form of mixed co-materials. Dioxins or furans may theoretically have 210 isomers depending on the number of chlorine atoms and the substituted position. In the present environment, about 130 species are detected.

≪ Formula 1 >

BRIEF DESCRIPTION OF THE DRAWINGS The above and other objects, features and advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which: FIG. In particular, the technical idea of the present invention and its core structure and action are not limited by this. In addition, the content of the present invention can be implemented by various other types of equipment, and is not limited to the embodiments and examples described herein.

A conventional pretreatment method of a sample for analyzing dioxin or furan is as shown in FIG.

FIG. 2 shows a pretreatment method of a sample according to the present invention. An appropriate amount of the collected dioxin or furan analytical sample was separated into filtrate and solid. The liquid phase was treated with a washing solution such as an inlet tube and an impinger, or with a diethylene glycol solution, and then extracted twice with 100 ml of toluene per 1 liter of washing solution. Solids were filtered through XAD-2 resin or cylindrical filter paper and Soxylat extracted with toluene for 16 hours or longer. (15 kinds such as ¹³ C12-2,3,7,8-T4CDD) was added to the extract of the sample which had been subjected to the extraction process of toluene and Soxhlet, and the mixture was concentrated to about 5 ml in a concentrator, To remove the functionalized toluene, and the mixture was concentrated to about 1 ml.

As shown in FIG. 3, a multi-layer silica gel column was prepared and washed with 50-150 ml of n-hexane. The concentrated sample was added to the washed column through a multilayer silica gel column and eluted with 150 ml of n-hexane. The solution was concentrated to about 5 ml in a concentrator, and then purged with nitrogen gas and concentrated to about 1 ml. The multi-layer silica gel column chromatography concentrate was subjected to alumina column fractionation with 70 ml of n-hexane containing 2% dichloromethane and 100 ml of a mixture of n-hexane: dichloromethane (1: 1).

The fractionation experiment was concentrated to a concentration of about 1 ml or less in a concentrator, and then concentrated to about 100 μl with nitrogen gas while maintaining the temperature at a constant temperature through a lower heating plate. Then, toluene was added to convert the solvent.

Alumina column fractionation The final concentrate was mixed with a certain amount of internal standard substance ( ¹³ C12-1,2,3,4-T4CDD, ¹³ C12-1,2,3,7,8,9-H4CDD) About 40 to 100 μl, and then 1 to 10 μl of the analytical sample solution was collected and injected and analyzed in a high-resolution gas chromatography or mass spectrometer.

In the purification process of the pretreatment method according to the present invention, the purification process of sulfuric acid for removing a large amount of organic substances from the extracted sample and the purification of the silica gel column for removing polar substances and coloring substances are performed to remove impurities , But the purification method using a multi-layer silica gel column (a multi-layer column) as the first step was adopted.

The multi-layer silica gel column may be packed in the order of neutral silica gel, potassium hydroxide silica gel, sulfuric acid silica gel, neutral silica gel, silver silver nitrate silica gel, anhydrous sodium sulfate, and copper particle layer. More preferably, the multilayered silica gel column is filled in the order of a neutral silica gel, a potassium hydroxide silica gel, a first sulfuric acid silica gel, a second sulfuric acid silica gel, a neutral silica gel, a silver silver nitrate silica gel, an anhydrous sodium sulfate and a copper particle layer, 1 sulfuric acid silica gel is 44% sulfuric acid silica gel, and the second sulfuric acid silica gel is 22% sulfuric acid silica gel.

The first sulfuric acid silica gel may have an average particle size of 100 to 150 mu m.

The second sulfuric acid silica gel is an alternative to the conventional sulfuric acid treatment and has an average particle size of 30 to 50 μm and may be filled at a ratio of 1.2 to 1.5 times as much as the first sulfuric acid silica gel.

Meanwhile, in the conventional method of concentrating the purified sample with nitrogen gas, in the concentration process of the pretreatment method according to the present invention, the sample extracted through the purification process is heated at a proper temperature, for example, 100 deg. C, more preferably 70 deg. C to 90 deg. C (in the case where the solvent is toluene).

That is, the pretreatment method of a sample for the analysis of dioxins or furans can be roughly divided into a purification process and a concentration process. In the present invention, by shortening the purification process, the time required is drastically shortened, It is imported.

Multilayer silica gel Column  Produce

A schematic diagram of a multi-layered silica gel column used in the present invention is shown in Figure 3 and comprises about 0.9 parts by weight of neutral silica gel, about 3 parts by weight of about 2% potassium hydroxide silica gel, about 0.9 parts by weight of neutral silica gel, about 44% About 4.5 parts by weight of a first sulfuric acid silica gel having an average particle diameter of 50 mu m, about 6 parts by weight of a 22% sulfuric acid silica gel (second sulfuric acid silica gel having an average particle diameter of 50 mu m), about 0.9 part by weight of a neutral silica gel, 6 parts by weight of anhydrous sodium sulfate, and about 1 part by weight of copper particles.

The major components used in the preparation of the multilayer silica gel column were prepared as follows. 40 g of 50 g / L KOH solution was added to 100 g of silica gel and mixed. The 2% potassium hydroxide silica gel which was decompressed, concentrated and dried at 50 DEG C was sealed and stored in a desiccator. 28.2 g and 78.6 g of sulfuric acid were added to 100 g of silica gel, and the 22% and 44% sulfuric acid silica gels were sealed and stored in a desiccator. 28 g of 400 g / L AgNO ₃ solution was added to 100 g of silica gel, and the 10% silver nitrate silver silica gel, which was decompressed, concentrated and dried at 50 ° C, was sealed in a brown glass bottle and stored in a desiccator.

A sample for analysis of dioxin or furan was injected into the above-mentioned multilayer silica gel column, and the sample was concentrated by ionizing it with 150 ml of a normal hexane solution. The recovery rates according to the amount of electrolytic solution are shown in Table 1. As a result, it was confirmed that the solution was sufficiently recovered by 120 ml of electrolytic solution.

Ion solution (ml) AG-1
100ml AG-2
10ml AG-3
10ml AG-4
10ml AG-5
10ml Recovery rate of standard substances for purification (%) 104.0 1.2 0.2 0.3 0.2

lunar caustic column  Fractionation experiment

As shown in Table 2, when the multi-layered silica gel column of the present invention was used to perform a fractional experiment of a sample containing silver nitrate, it was confirmed that the extract was sufficiently recovered when 150 ml of a normal hexane solution was ionized using a multilayer silica gel column there was.

division Chlorine water Analysis item AG-1 AG-2 AG-3 AG-4 AG-5 Pew
Ran 4 ¹³ C ₁₂ -2,3,7,8-TCDF 112.1 0.6 0.0 0.3 0.0 5 ¹³ C ₁₂ -1,2,3,7,8-PeCDF 98.0 0.7 0.2 0.4 0.0 ¹³ C ₁₂ -2,3,4,7,8-PeCDF 99.9 0.8 0.0 0.0 0.0 6 ¹³ C ₁₂ -1,2,3,4,7,8-HxCDF 102.3 1.0 0.3 0.3 0.0 ¹³ C ₁₂ -1,2,3,6,7,8-HxCDF 109.3 0.9 0.0 0.3 0.0 ¹³ C ₁₂ -2,3,4,6,7,8-HxCDF 103.6 0.0 0.0 0.0 0.0 ¹³ C ₁₂ -1,2,3,7,8,9-HxCDF 114.9 1.4 0.0 0.0 0.0 7 ¹³ C ₁₂ -1,2,3,4,6,7,8-HpCDF 116.7 1.3 0.0 0.2 0.1 ¹³ C ₁₂ -1,2,3,4,7,8,9-HpCDF 115.7 2.3 0.0 0.0 0.0 All
this
jade
God 4 ¹³ C ₁₂ -2,3,7,8-TCDD 94.8 0.5 0.0 0.2 0.1 5 ¹³ C ₁₂ -1,2,3,7,8-PeCDD 86.1 0.8 0.0 0.0 0.0 6 ¹³ C ₁₂ -1,2,3,4,7,8-HxCDD 97.2 0.7 0.0 0.3 0.2 ¹³ C ₁₂ -1,2,3,6,7,8-HxCDD 111.3 1.0 0.0 0.3 0.2 7 ¹³ C ₁₂ -1,2,3,4,6,7,8-HpCDD 95.8 3.2 0.0 2.3 0.0 8 ¹³ C ₁₂ -OCDD 102.5 2.6 0.0 0.1 0.0 medium(%) 104.0 1.2 0.2 0.3 2.0 Maximum value 116.7 3.2 2.3 3.2 2.0 Minimum value 86.1 0.0 0.0 0.0 0.0

Alumina column  Fractionation experiment

Separation of 2% and 50% Methylenechloride in Hexane used in refining alumina was carried out 7 times (20, 30, 40, 50, 70, 80ml) and 5 times (30, 60, 90, 120, 150ml) (Fractionation) experiment. As a result, it was confirmed that the recovery rate was the maximum value when 70 ml of 2% Methylenechloride in Hexane and 90 ml of 50% Methylenechloride in Hexane were flown.

Validation of the method according to the invention

The sample was eluted with 150 ml of a normal hexane solution using the above-mentioned multilayer silica gel column, and purified by flowing 70 ml of 2% Methylenechloride in Hexane and 90 ml of 50% Methylenechloride in Hexane through an alumina column. The purified extract was concentrated using a nitrogen gas in a state where a heating plate was provided at the lower part and the temperature was maintained at an appropriate temperature. The final concentrate was analyzed using a high resolution gas chromatograph or mass spectrometer.

As shown in Table 3, it was confirmed that the measurement values of the incineration-related samples and the soil-related samples were within ± 1σ of the standard deviation.

Field Name of sample Measures
Incineration-related samples (ng-TEQ / g) Asha 0.19 Ash B 2.44 Ash C 0.19
Soil-related samples (ng-TEQ / g) Soil S 0.065 Soil B 0.442 Soil C 0.515 Soil D 0.078

As shown in Table 4 and Table 5, it is confirmed that the value is similar or slightly lower than the expected value.

Dioxin or Furans Analysis item Expected value Measures Reference drawing Pew
Ran 2,3,7,8-TCDF 25 27 6 1,2,3,7,8-PeCDF 25 25 7 2,3,4,7,8-PeCDF 25 25 8 1,2,3,4,7,8-HxCDF 50 50 1,2,3,6,7,8-HxCDF 50 50 2,3,4,6,7,8-HxCDF 50 56 1,2,3,7,8,9-HxCDF 50 50 1,2,3,4,6,7,8-HpCDF 50 51 1,2,3,4,7,8,9-HpCDF 50 50 OCDF 125 131 12 All
this
jade
God 2,3,7,8-TCDD 25 27 13 1,2,3,7,8-PeCDD 5 26 2,3,4,7,8-HxCDD 50 56 1,2,3,6,7,8-HxCDD 50 55 1,2,3,7,8,9-HxCDD 50 52 1,2,3,4,6,7,8-HpCDD 50 48 15 OCDD 125 125 16

Co-PCB Analysis item Expected value Measures PCB # 77 16 11 PCB # 126 16 12 PCB # 19 16 12 PCB # 81 32 23 PCB # 105 16 11 PCB # 114 16 11 PCB # 118 32 23 PCB # 123 16 12 PCB # 156 32 24 PCB # 157 16 12 PCB # 167 16 12 PCB # 189 16 12

As described above, the present invention simplifies the pretreatment process of the sample for analysis of dioxin or furan by pretreating the sample using the multilayer silica gel column, thereby reducing the processing time and dramatically reducing the analysis reagent.

While the present invention has been particularly shown and described with reference to specific embodiments thereof, those skilled in the art will appreciate that such specific embodiments are merely preferred embodiments, It will be obvious. It is therefore intended that the scope of the present invention be defined by the appended claims and their equivalents.

Claims (7)

(a) an extract preparation step of extracting dioxin or a furan-containing extract from a sample using a solvent;
(b) a first concentrate preparation step of removing the solvent from the extract;
(c) a primary chromatographic step of fractionating said primary concentrate using a multi-layered silica gel column;
(d) a second concentrate preparation step for concentrating the fraction after the first chromatography step;
(e) a second chromatographic step of fractionating the second concentrate using a column packed with alumina; And
(f) obtaining a sample for analysis by concentrating the fraction through the secondary chromatography step,
The multilayer silica gel column was prepared by mixing 0.9 part by weight of neutral silica gel, 3 parts by weight of 2% potassium hydroxide silica gel, 4.5 parts by weight of 44% of primary sulfuric acid silica gel, 6 parts by weight of secondary sulfuric acid silica gel of 22%, 0.9 parts by weight of neutral silica gel, % Silver nitrate silver silica gel 3 parts by weight, anhydrous sodium sulfate 6 parts by weight and copper particles 1 part by weight layer,
The first sulfuric acid silica gel has an average particle size of 110 mu m, the second sulfuric acid silica gel has an average particle size of 50 mu m,
The solvent is toluene,
Wherein the step of obtaining the sample is performed while heating at a temperature of 70 to 90 占 폚 in a nitrogen atmosphere, and then the concentrated sample is subjected to a pretreatment method of the sample for dioxin or furan analysis.
delete delete delete delete A method for analyzing dioxin or furans, which comprises injecting a sample pretreated by the method of claim 1 into a high-resolution gas chromatograph or mass spectrometry.





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