KR102026070B1 - Method of identifying origin of hot pepper powder using optical microscope - Google Patents

Abstract

The present invention relates to a method for determining whether red pepper powder is derived from frozen red pepper using an optical microscope, which comprises the steps of: (a) selecting a piece of red pepper powder (having a skin layer attached thereto and a size of 2×2 mm or more) in which a segment operation can be performed from a red pepper powder sample; (b) forming a segment of the red pepper powder by cutting the piece of the red pepper powder by the thickness of 0.1 mm or less using a scalpel; (c) placing the segment of the red pepper powder on a slide glass, dropping one drop of triethanolamine, and swelling the segment in the triethanolamine for 3 to 5 minutes; and (d) performing methylene blue dyeing on the swollen segment, and observing the same with an optical microscope to determine whether the swollen segment is derived from a frozen red pepper.

Description

Method of identifying origin of hot pepper powder using optical microscope}

The present invention relates to a method for discriminating whether or not frozen pepper is derived from chilled pepper using an optical microscope, and more specifically, whether the dried pepper has undergone a freezing process before being processed into red pepper powder by observing the cross-sectional structure of frozen pepper powder using an optical microscope. It relates to a method of determining whether or not.

According to Article 6 (Prohibition of False Labels, etc.) of the Act on the Labeling of Country of Origin of the Current Agricultural and Fishery Products, paragraph 1 (1) of the Importer of agricultural and marine products or its processed products, which are produced, processed and shipped or sold (including mail order) A person who keeps or displays for the purpose of selling or selling is not to make a "false or confusing indication of origin".

In addition, a person who violates this may be subject to imprisonment of not more than seven years or a fine not exceeding 100 million won or in accordance with Article 14 (Penalty) of Chapter 4 of the Act on Labeling of Country of Origin of Agricultural and Marine Products. It is prescribed.

At present, the price of domestic and Chinese red pepper powder is more than twice as high as the domestic price. Some manufacturers and distributors use red pepper powder mixed with domestic or Chinese to produce the origin of Chinese red pepper powder for the purpose of gaining unfair profit. The country of origin is sold falsely labeled as domestic.

However, the red pepper powder cannot be identified by the naked eye, and the red pepper powder is identified by the origin identification method of red pepper powder using inductively coupled plasma spectroscopy (ICP), a conventional red pepper powder origin assay method (Patent Literature 1, Non-Patent Literature 1) and near-infrared spectroscopy. The method of discriminating the origin and pepper seed mixture of non-patent literature (Non-Patent Literature 2) is a statistical test, and the causal relationship between the test results cannot be clearly explained, and thus the evidence of pepper powder origin test results is problematic in the trial process. Therefore, the suspects who abuse it deny all charges of false labeling of the origin of the red pepper powder, and the crackdown officials also passively endeavor to crack down on the red pepper powder of the origin labeling.

Meanwhile, May 2018. Currently, domestic red pepper powder retail price is about 20,000 won / kg, and Chinese red pepper powder is about 10,000 won / kg, which is twice as expensive as domestic products, so the origin of Chinese red pepper powder is highly likely to be domestic.

For this reason, cheap Chinese red pepper powder is frequently distributed in domestic production, while there is no proper way of controlling red pepper powder, so the willingness of domestic dried red pepper producers is becoming weaker. Therefore, red pepper powder is also used to protect domestic dried red pepper producers. It is urgent to establish a method of control of origin.

Korea Patent Publication No. 10-1742606

 Korean Society of Analytical Science, Fall Conference, pp.219-219, (2016.11)  Journal of Oil and Applied Sciences, Vol. 16 No.2, pp.155-161 (1999)

The present invention has been made in order to solve the above problems, an object of the present invention is to observe the red pepper powder unit using an optical microscope to determine whether the pepper powder produced through the freezing process to determine whether the red pepper powder using an optical microscope It is to provide a method for determining whether pepper is derived.

The present invention to achieve the above object, (a) selecting the red pepper powder from the red pepper powder sample, (b) cutting the selected red pepper powder to obtain a red pepper powder slice, (c) the red pepper powder slice Placing on a slide glass and dropping triethanolamine, swelling the red pepper flakes, and (d) treating the swollen red pepper flakes with methylene blue staining, then observing with an optical microscope to determine whether frozen pepper originated. It includes a, provides a method for determining whether the frozen pepper derived of red pepper powder using an optical microscope.

According to the present invention, since it is possible to determine whether or not the red pepper powder processed by frozen pepper to determine whether the origin of the red pepper powder is violated, by actively utilizing the method according to the present invention to control the illegal distribution of red pepper powder, the red pepper powder originated by eliminating the illegal distribution of red pepper powder It will be able to prevent cheating that low priced red pepper powder becomes domestic, stabilize the price of domestic red pepper powder, inspire the willingness of domestic pepper producing farmers, and ensure that high quality domestic high quality red pepper powder is safely supplied to the market to improve customer satisfaction. .

Figure 1a is a scene containing about 10g of pepper powder to be observed in the sample dish.
1B is a scene of selecting a piece of pepper powder capable of cutting.
1C is a scene of making pepper powder slices using a mass.
1D is a scene in which a red pepper powder slice is placed on a slide glass.
FIG. 1E is a scene in which 1 drop of Triethanolamine is dropped on a red pepper powder slice.
1f is a scene in which 1 drop of methylene blue is dropped onto a red pepper powder swelled with triethanolamine.
Figure 1g is a scene observing the stained red pepper slices under a microscope.
Figure 1h is a 100 times magnification of the red pepper slices with an optical microscope.
Figure 1i is a 100 times magnified image of the red pepper powder swelled in Triethanolamine with an optical microscope.
Figure 1j is a 100 times magnified image of the red pepper powder stained with methylene blue (light blue) by an optical microscope. The photo on the left is Korean red pepper powder, and the photo on the right is frozen red pepper powder from China. In the left domestic pepper powder, the cell structure of the inner red pepper powder (B · C) is observed without distortion, but in the right Chinese red pepper powder, the cavitation (phenomena due to the destruction of the cell wall) is observed in the inner red pepper powder (B). .
Figure 1k is a 100 times magnified image of the red pepper powder stained on methylene blue (Methylene blue) with an optical microscope. The photo on the left is Korean red pepper powder, and the photo on the right is frozen red pepper powder from China. In the left domestic red pepper powder, the cell structure of the inner red pepper powder (B · C) is observed without deformation, but in the right red pepper powder, the cavitation (phenomena caused by the destruction of the cell wall) occurs in the inner red pepper powder (B · C). Is observed.
Figure 2a is a scene of putting about 50g of cabbage kimchi in a sample of cabbage kimchi into a beaker containing 200ml of water. This is to separate the kimchi (seasoning) from the cabbage kimchi with water.
Figure 2b is a scene to take out the cabbage washed in water.
Figure 2c is a scene separating the kimchi (season) and water with a 1mm mesh.
2d is a scene in which red pepper powder in kimchi is spread on a gauze on a mesh.
2E is a scene where kimchi (seasoning) is placed in a food dryer.
Figure 2f is a scene of drying the kimchi (seasoning) with a food dryer.
2g is a scene of making red pepper powder slices using dried red pepper powder in kimchi.
Figure 2h is a scene observing the pepper powder slices in kimchi with an optical microscope.
Figure 2i is a 100 times magnified image of the domestic chili powder in kimchi with an optical microscope.
Figure 2j is a 100 times magnified image of Chinese red pepper powder in kimchi with an optical microscope.

The present invention comprises the steps of: (a) selecting the red pepper powder from the red pepper powder sample, (b) cutting the selected red pepper powder to obtain red pepper powder slices, (c) placing the red pepper powder slices on a slide glass and dropping triethanolamine Swelling the red pepper powder slices, and (d) subjecting the swollen red pepper powder slices to methylene blue staining, and then observing with an optical microscope to determine whether frozen peppers are derived from red pepper powder using an optical microscope. It relates to a method of determining whether or not derived from frozen pepper.

In the step (a) of the method of determining whether the red pepper powder is derived from frozen pepper according to the present invention, the red pepper powder has an epidermal layer, and may have a size of 2 × 2 mm or more, preferably 2 × 2 mm to 5 × 5 mm. . This is to screen out red pepper pieces that can be sliced.

In the method of determining whether the red pepper powder is derived from the frozen pepper of the present invention, the step (b) may be a step of obtaining a red pepper powder slice by cutting the selected red pepper powder to a thickness of 0.1 mm or less using a mass.

In the method of determining whether the red pepper powder is derived from the frozen red pepper of the present invention, the step (c) places the red pepper slices on a slide glass and drops 1 drop of triethanol amine, and the mixture is left for 3 to 5 minutes. Swelling the red pepper slices.

In the step (d) of the method of determining whether the red pepper is derived from the frozen pepper of the present invention, as a result of the optical microscope, the sample showing the cavitation in which the cellular tissue of the red pepper powder inner layer is destroyed and the hole is formed is derived from the frozen red pepper. Can be determined.

In the step (d) of the method of determining whether the red pepper is derived from the frozen pepper of the present invention, the optical microscopic observation reveals that the sample showing the voids caused by the destruction of the cellular structure of the red pepper inner layer is made in China. Samples that do not appear can be identified as Korean.

Chinese dried red pepper, which is distributed at low cost in Korea, is mostly frozen red pepper (raw red pepper) harvested from China and imported to Korea and dried at domestic drying facilities, and Chinese red pepper powder is made from Chinese dried red pepper. It is processed with red pepper powder.

In China, the red pepper (raw pepper), which is not frozen or red pepper, is imported into Korea because the tariff rate of red pepper (raw pepper) is 27%, while the dry and red pepper powder tariff rate is 270%. This is due to the operating margin of importers.

On the other hand, unlike domestic Chinese, the dried red pepper was dried immediately after harvesting, without going through the freezing process, and the difference between the domestic dried pepper and Chinese dried pepper can be confirmed by the presence of the freezing process. The characteristics of dried red peppers by origin are clearly shown. Domestic dried red peppers have a smooth surface, while Chinese dried red peppers have a trace of hardened substance inside the pepper during freezing.

If you observe the dried Chinese pepper without freezing process and the Chinese dried pepper after freezing process, you can observe the dense cell tissue in the cross section of the Korean dried red pepper, Cell wall destruction due to volume expansion due to freezing) is observed, and this phenomenon is also reflected in the red pepper powder of each origin processed with the above raw materials, and the cross section of red pepper powder is observed using an optical microscope to determine the destruction of cellular tissue and freeze it. It is possible to check whether the red pepper powder originated from the dried red pepper is processed and to use it as evidence of violation of the origin labeling, thus contributing to establishing the distribution order by preventing the cheating of the red pepper powder origin.

In particular, red pepper powder processed with Chinese frozen dried pepper is mostly used to make kimchi in Chinese cabbage kimchi manufacturers and restaurants.However, there was no proper origin test method for the red pepper powder in kimchi, so 'the method to determine whether frozen pepper is derived from red pepper powder using optical microscope' May be a useful alternative to the red pepper powder origin assay in kimchi.

Hereinafter, the present invention will be described in detail with reference to the drawings.

1a to 1b is a scene that screens the slices of pepper powder that can be sliced from the red pepper powder sample, the slices of pepper powder that can be sliced is 2 × 2mm or more and the epidermal layer is attached. For the above sorting operation, a sieve size 2.0mm mesh can be used, and the amount of sample required for sorting is about 10g, and about 20 pieces of red pepper powder are selected for each sample.

Figure 1c is a scene of making a pepper powder slice using a mass of the selected pepper powder. The thickness of red pepper slice should be 0.1mm or less so that the internal tissue morphology can be clearly observed when microscopically observed. Make pepper slices for each piece of pepper powder you select.

1D is a scene where the red pepper powder is placed on a slide glass. 20 pepper powder slices are made for each sample and placed on slide glass.

Figure 1e is a scene of dropping one drop of Triethanolamine (red pepper flakes). Pepper powder slices swell in Triethanolamine and return to about 80% of their dry state in about 3 to 5 minutes.

FIG. 1F is a scene in which 1 drop of methylene blue is dropped onto the swollen pepper powder slice. Methylene blue staining treatment before optical microscopy can clearly observe the internal structure of red pepper.

Figure 1g is a scene observing the stained red pepper slices with an optical microscope. The optical microscope magnification is 100x and the model used is LEICA DM750.

Figure 1h is a photograph of the red pepper powder before triethanolamine treatment, Figure 1i is a photograph of the red pepper powder after triethanolamine treatment.

Figure 1j is a 100 times magnified image of the red pepper powder stained with methylene blue (light blue) by an optical microscope. The photo on the left is Korean red pepper powder, and the photo on the right is frozen red pepper powder from China. In the left domestic pepper powder, the cell structure of the inner red pepper powder (B · C) is observed without distortion, but in the right Chinese red pepper powder, the cavitation (phenomena due to the destruction of the cell wall) is observed in the inner red pepper powder (B). .

Figure 1k is a 100 times magnified image of the red pepper powder stained on methylene blue (Methylene blue) with an optical microscope. The photo on the left is Korean red pepper powder, and the photo on the right is frozen red pepper powder from China. In the left domestic red pepper powder, the cell structure of the inner red pepper powder (B · C) is observed without deformation, but in the right red pepper powder, the cavitation (phenomena caused by the destruction of the cell wall) occurs in the inner red pepper powder (B · C). Is observed.

 In the photograph of the red pepper powder of FIGS. 1J to 1K, 'A' is a pepper skin layer, and 'B · C' is a pepper inner layer. Comparing the cross section of domestic red pepper powder with the cross section of Chinese red pepper powder, there is no change in the 'A' layer, but different shapes can be observed in the 'B · C' layer. The reason why the cavitation of the 'B · C' layer occurs in frozen pepper is interpreted as 'cell wall destruction by volume expansion of water due to freezing'.

1A to 1K illustrate a method for determining dried frozen peppers of red pepper powder using an optical microscope. 20 pieces of red pepper powder are selected for each red pepper powder sample, and each piece of red pepper powder that can be observed under an optical microscope is selected from the selected red pepper pieces.

The observer microscopic observation of the 20 pieces of pepper powder to determine the destruction of the 'B · C' layer, and determines how much the frozen pepper is mixed in the pepper powder sample. In this way, it is possible to check how much Chinese frozen pepper is mixed with the red pepper powders requested.

Figure 2a is a scene of putting about 50g of cabbage kimchi in a sample of cabbage kimchi into a beaker containing 200ml of water. This is to separate the kimchi (seasoning) from the cabbage kimchi with water.

Figure 2b is a scene to take out the cabbage washed in water.

Figure 2c is a scene separating the kimchi (season) and water using a 1mm mesh. The mesh used in the experiment was Cheongggye Construction 1.0mm No. 18.

Figure 2d is a scene of spreading the kimchi inside (seasoning) gauze filtered over the mesh.

2E is a scene where kimchi (seasoning) is placed in a food dryer.

Figure 2f is a scene of drying the kimchi (seasoning) with a food dryer. When dried in a food dryer for 2 to 4 hours, it is dried to 15% or less of moisture. The food dryer used for the experiment used SFD-H480M model of Shinil Industry Co., Ltd.

Figure 2g is a scene of making pepper powder slices using a mass to remove the pepper powder that can be sliced in the dried kimchi (seasoning). Hereinafter, the experiment procedure and method are the same as those of Figs. 1a to 1k, which are a method for discriminating dried chilled pepper of red pepper powder using an optical microscope.

Figure 2h is a scene observing the pepper powder in kimchi with an optical microscope. The microscope model, conditions, and observation method used in the experiment are the same as the above-described method for determining dried frozen peppers of red pepper powder using an optical microscope.

2i is a photograph of a 100 times magnification of Korean red pepper powder in kimchi with an optical microscope.

Figure 2j is a 100 times magnified photograph of Chinese red pepper powder in kimchi with an optical microscope.

Hereinafter, the present invention will be described in detail by examples. However, the following examples are merely to illustrate the invention, the scope of the present invention is not limited thereto.

< Example 1> optical microscope  Determination of the Origin of Frozen Red Pepper Using Red Pepper Powder

In the method of discriminating the dried chilli pepper of red pepper powder using an optical microscope, pour about 10g of red pepper powder to be tested on the sample dish, and then select 20 pieces of red pepper powder that have a red pepper epidermis layer and the size of 2 × 2mm or more, Red pepper flakes having a thickness of 0.1 mm or less were obtained.

Put the red pepper slices on the slide glass and drop 1 drop of triethanolamine and wait for about 3 ~ 5 minutes.The red pepper powder swells to 80% before drying, and after dropping 1 drop of methylene blue, observe it with an optical microscope. As a result of determining the presence of layer breakage (cavitation) to determine whether or not frozen peppers are shown in Table 1 below.

Domestic red pepper cross-section photo Chinese red pepper powder cross-section picture

채취일: 2017.2.6., 춘천닭갈비 (전남 순천시)

Date of Harvest: Feb. 2017, Chuncheon Chicken Ribs (Suncheon, Jeonnam)

Date of Collection: April 4, 2017, Haesong Restaurant (Suncheon, Jeonnam)

Collection Date: March 2, 2017, Jeollado Surgical Prize (Gwangyang-si, Jeonnam)

Date Harvested: May 20, 2017, Ribs per Second (Jeosu, Jeonnam)

Date Collected: Jun. 2017, Bear Cattle (Iksan-si, Jeonbuk)

Date Picked: 2017.7.6., Pepper Country (Gyeongsan, Gyeongbuk)

Date of Collection: July 6, 2017, Chilli-Nara (Gyeongsan, Gyeongbuk)

Collection Date: Aug. 2, 2017, Jinwoong Food (Anseong, Gyeonggi)

Date of Collection: Aug. 2018, Cheong Lim, Jeongeup-si, Jeonbuk

Collection Date: Feb. 2018, Daesung Foods (Daejeon)

Date of Harvest: Apr. 2, 2018, Joongang Rice House (Haenam-gun, Jeonnam)

Date of Harvest: Apr. 2018, Achieved Agriculture (Chungju, Chungbuk)

Comparing the cross-sectional photographs of the red pepper powder according to the origin of Table 1, in the domestic red pepper powder, the cells inside the red pepper are observed without being destroyed, but in Chinese red pepper powder, it can be observed that a crack occurs vertically in the red skin layer of the red pepper. In other words, Chinese red pepper powder during the freezing process of the red pepper destroys the cell wall inside the pepper, while domestic pepper powder, such a phenomenon is not observed, it can be used to crack down on the red pepper powder origin.

< Example  2> Optical microscope  Discrimination of Frozen Chili Pepper from Kimchi

The method of discriminating frozen peppers of red pepper powder in kimchi using optical microscope is to put kimchi about 50g into a beaker containing 200cc of water, separate the kimchi (seasoning) from the kimchi, and then use the mesh (1.0mm) Water was separated.

After spreading the kimchi (seasoning) on the gauze on the mesh, it was put in a food dryer and dried to have a water content of 15% or less for 2 to 4 hours.

After selecting the pieces of red pepper powder in the dried kimchi (seasoning), the red pepper powder was made by the same process as in Example 1 and observed with an optical microscope to determine whether the frozen pepper.

Although the present invention has been described in detail with reference to specific embodiments, the present invention is not limited to the above-described embodiments, and many modifications are made by those skilled in the art to which the present invention pertains within the scope of the technical idea of the present invention. This possibility will be self-evident.

The present invention is a method for determining whether raw material dried pepper has undergone a freezing process by observing red pepper powder cell tissue under an optical microscope, and can quickly and accurately determine whether it is red pepper powder derived from frozen red pepper, and also removes red pepper powder in kimchi. Since there is an advantage that can be determined, it can be usefully applied to the technical field to which the present invention belongs.

In addition, this determination method is expected to contribute to the eradication of fraudulent distribution of agricultural products by discriminating even red pepper powder of frozen red pepper, and even frozen agricultural products.

Claims (6)

(a) screening the red pepper powder pieces from the red pepper powder sample;
(b) cutting the selected red pepper powder to obtain red pepper powder slices;
(c) placing the red pepper flakes on a slide glass and dropping triethanolamine to swell the red pepper flakes; And
(d) after the methylene blue staining treatment on the swelled red pepper powder slice, by observing with an optical microscope to determine whether or not derived from the frozen pepper, the method of determining whether frozen pepper originated from red pepper powder using an optical microscope. The method of claim 1, wherein in the step (a), the red pepper powder is attached to the epidermis layer and has a size of 2 × 2 mm or more. [Claim 2] The method of claim 1, wherein the step (b) determines whether the red pepper powder is derived from the chilled pepper powder using an optical microscope, wherein the selected red pepper powder is cut to a thickness of 0.1 mm or less using a mass to obtain a red pepper powder slice. . The optical microscope of claim 1, wherein the step (c) comprises placing the red pepper flakes on a slide glass, dropping 1 drop of triethanolamine, and leaving the mixture for 3 to 5 minutes to swell the red pepper flakes. How to determine whether the red pepper is derived from the chilled pepper used. According to claim 1, wherein the optical microscope observation step in the step (d), the cell tissue of the inner layer of red pepper powder appears to appear a cavity cavitation occurs in the sample showing the optical microscope, characterized in that derived from the frozen pepper How to determine whether the red pepper is derived from the chilled pepper used. According to claim 1, wherein the optical microscope observation step in the step (d), the cell tissue of the inner layer of the red pepper powder is destroyed, the sample showing the cavity is made in China, the sample does not appear the cavity is determined to be made in Korea Method for determining whether or not derived from the chilled pepper of red pepper powder using an optical microscope.

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