KR100806539B1 - The identification method of Angelica gigas Nakai origin - Google Patents

Abstract

The present invention relates to a method for identifying a Angelica origin.

Todanggwi that grows in the country (Angelica gigas) is the scientific name is the main ingredient in 'Angelica gigas Nakai' is Decursin, was being Decursinol containing much scientific name of ildanggwi (why Angelica) is the main ingredient in 'Angelica acutiloba kitagawa' is a VB ₁₂ Chinese Angelica's scientific name is 'Angelica acutiloba kitagawa' and its main ingredient is VB ₁₂ . As described above, the conventional identification method of the donkey is made by the naked eye, but in the present invention, a method of identifying a scientific origin through analysis by advanced analysis equipment, decursin, which is a main component specifically detected only in true donkey, According to the presence or absence of decursinol, if it is not detected, it is determined to be imported. The assay is optimized for extraction by accelerated solvent extraction (ASE) at a temperature of 80 ° C, a pressure of 1500psi, and a solvent in n-Hexane. The present invention relates to a method for identifying a donkey origin.

Donkey, origin, identification, method

Description

The identification method of Angelica gigas Nakai origin}

Figure 1 is a substitute picture of Angelica gigas.

Figure 2 is a drawing substitute picture of the import donkey.

Figure 3 is a process diagram of the country of origin identification carried out by the National Agricultural Products Quality Management Service.

The present invention relates to a method for identifying a Angelica origin.

Todang (Suddock), which is native to Korea, is the medicinal name of Seunggeumcho's root, its scientific name is' Angelica gigas Nakai ', and its properties are' 辛 (신), 苦 (고), 溫 (')'. And the scientific name of Dangdang-Gui (Dang-Dong-Gui), which is imported and grown for export purposes in Japan, is called `` Angelica acutiloba kitagawa '' and its properties are `` (Persimmon), 辛 (Shin), 溫 (On) '. It contains a lot of VB ₁₂ , and its scientific name is Angelica acutiloba kitagawa, and its properties are 감 ()), 微 (미), 辛 (신), 溫 (온), and the main component is VB _12. There are many contained features.

Dongguk is a crop that does not like crops, and it is mainly cultivated in the mountainous and cold regions of the northern and northern regions.

The cultivated area gradually decreased to 2,344 ha in '95, 1,035 ha in '98, and 988 ha in '99, and then increased to 1,016 ha in 2000 and 1,282.7 ha in 2002.

According to the Korea Herbal Medicines Association, the output was 2,214 tons in '89, 3,243 tons in '92, and 7,044 tons in '95, but the average number of plants decreased. Is reported at 3,342 tons, and 3,523 tons in 2004.

The use site is the root, and the tang Dung is a pharmacological function of uterine function control, sedation, pain relief, diuresis, vitamin E deficiency treatment, antibacterial action, hypothalamic action. Is a tonic tonic used for the treatment of anemia, postpartum care, and pain medication.

The price is 6,820 won per day, compared to 4,210 won per day for 600g. So, the price of donkey ear is better for export and profitability.

As described above, although the price difference is high for each country of origin, it is not easy to identify the country of origin with the naked eye, but the Angelica Angelica has a large slice and a lot of mixed roots, but the imported product has a large slice and a few small roots.

Shells are light yellowish brown to dark brown with dark yellow inner shell, white in center, while imported shells are light brown in color and slightly white in yellow.

In addition, as shown in the accompanying drawings, a real donkey has no wire holes to be rolled up without using wires (FIG. 1), but imported wires are sewn with wires to dry out. (FIG. 2)

Currently, the purpose of identification of the country of origin under the Agricultural Products Quality Control Act is to prevent the illegal distribution and establish a sound distribution order to protect the producers and consumers by conducting the origin verification through the research and development of the scientific origin identification method to establish the origin labeling system. have.

The verification step (Fig. 3) for origin identification performed by the National Institute of Agricultural Products Quality Management in Korea (Fig. 3) is' sample reception-sample pre-processing-specific sample analysis (NIRS, ICP / MS, image analysis, E-NOSE, DNA analysis, XRF) -analysis result-origin determination '.

The country of origin identification by NIRS (Near Infra Red Spectrometer) analyzes the organic component content of the sample by absorbance energy value using near infrared wavelength (800 ~ 2,500nm), and then forms the standard calibration equation for each country to identify the country of origin. This is an experimental calibration technique that predicts the results of unknown samples using known samples.

 In addition, the country of origin identification by the E-NOSE (electronic Nose) is a method of analyzing the fragrance component of the sample by an electrical resistance value using a special sensor, and then identifying the country of origin by creating a database of characteristics of each country. Recently, Dr. Hyun-Joo Son, Ginseng and Tobacco Research Institute, has introduced electronic noses to screen domestic and Chinese ginseng.

The electronic nose contains twelve metal oxide sensors that react with volatile molecules that cause odors. When electronic nose takes ginseng fragrance, Chinese and Korean ginseng fragrance appear in distinct pattern on coordinates.

Origin identification by XRF (X-Ray Fluorescence Spectrometer) is a method of identifying the origin by analyzing the inorganic element content in the sample by irradiating X-rays on the sample.

Origin identification by DNA analysis is different from each other in the DNA structure, there is a method of identifying the origin by analyzing the nucleotide sequence of the amplified DNA by amplifying the gene using PCR.

The present invention is to provide a method for scientifically identifying the country of origin through analysis by advanced analysis equipment, apart from the conventional method of identifying the donkey by the naked eye, as described above.

In order to achieve the above object, an embodiment of the present invention is as follows.

EXAMPLE

Materials and methods

Material

1) Sample used

First, 116 samples of Angelica gigas and 88 imported samples from Korea.

2) test equipment

Accelrated Solvent Extractor (Model ASE200, Dionex, USA)

Gas Chromatograph (Model Agilent 6890 series, Agilent Technologies, USA)

B. Test Method

1) Sample pretreatment

Sample Collection: 100g per sample

Grind to -50 mesh and use 2g as sample.

2) Sample analysis

① Analysis principle:

The main components were different in the domestic and imported donkeys, and the origin was identified according to the presence or absence of specific components.

For reference, the main components by country of origin are shown in Table 1 below.

Mountain main ingredient Domestic Angelica Decursin, Decursinol Chinese donkey VB ₁₂ Japanese dwarf donkey VB ₁₂

Therefore, the results of analysis by the detection of Decursin, Decursinol (Decursinol), the main components of the true donkey with the sample is shown in Table 2 below.

According to the results of the analysis, decursin and decursinol components were detected in 116 samples of Korean Angelica gigas, but not in 87 of 88 imports. The reason for the analysis of mixed components of imported products was provided by the National Institute of Agricultural Products Quality Testing and Research Institute, and the sample was determined to be imported after identification of the first place of origin by E-NOSE, but the reliability level of electronic nose was 95%. In consideration of this, one point of uncertainty was excluded from the subject of sample review.

Therefore, it can be seen that the criteria for identifying the origin of Angelica must be based on the detection of decursin and decursinol components.

Therefore, the ASE extraction process for the prepared sample is as follows.

②ASE extraction process

-Fill the extraction cell (33ml) with one cellulose filter, 2g of sea sand, 4g of chem tube hydromatrix, 2g of sample, 4g of chem tube hydromatrix, and 2g of sea sand in order. The solution is extracted under conditions of 1 minute preheating, 5 minutes heating, 5 minutes settling time and 60% solvent flush.

As described above, in order to analyze the components that are specifically detected in true donkey, the present invention was examined the optimal extraction conditions of the domestic donkey specific component by accelerated solvent extraction (ASE).

Accelerated solvent extraction is used to extract residual pesticides or organics from solid samples. It is an automated analytical processing equipment that extracts organics from existing organic solvents under conditions of heating and pressurization. Decursin and Decursinol components were extracted for optimum conditions.

The analysis data carried out according to the temperature, pressure and solvent are shown in Tables 3, 4 and 5 below.

Temperature collection Decursinol Decursin system  Average amount of extraction  40 ℃ One 106506.8 82074.1 188581  187693 2 105229.9 82044.7 187275 3 106001.6 81222.5 187224  60 ℃ One 127463.7 95130.4 222594  221723 2 125643.7 93675.2 219319 3 127961.5 95295.1 223257  80 ℃ One 210234.6 156721 366956  371621 2 213483.3 159127.2 372611 3 215184 160112.2 375296  100 ℃ One 181205.7 133429.3 314635  318980 2 184141.7 135507.2 319649 3 185889.1 136767 322656  120 ℃ One 178607 134647.9 313255  194757 2 176401.8 133027.4 309429 3 177508.4 133893.9 311402

pressure collection Decursinol Decursin system  Average amount of extraction  500 psi One 109230.4 81909.6 191140  194757 2 112982 84690.12 197672 3 111703.7 82754.3 195458  1000 psi One 140027.8 103988 244016  250024 2 143849.4 106745.3 250595 3 146650.7 108809.6 255460  1500psi One 225673.1 168335 394008  387887 2 226161.1 168748.1 394909 3 214583.7 160160 374744  2000 psi One 192843.2 146279.9 339123  347055 2 199875.3 151397.2 351273 3 199471.2 151298.8 350770  2500psi One 149458.4 112508.8 261967  258016 2 149788.9 112808.1 262597 3 142333.9 107151.2 249485

menstruum collection Decursinol Decursin system  Average amount of extraction  hexane One 144493.6 110214.8 254708  265689 2 164597.7 125288.2 289886 3 143154.7 109317.5 252472 dichloromethane One 76877.4 5113.8 131991  132738 2 77452.7 55583 133036 3 77560.7 55627.1 133188 acetonitrile One 17620.2 12886.9 30507  30663 2 17738.9 13015.2 30754 3 17723.4 13005.2 30729

The above table of data on temperature, pressure, and solvent is shown in Tables 6, 7, and 8, respectively.

③ GC Analysis

As described above, to determine whether the decursin, decursinol component is detected in the solution for each sample extracted with ASE is subjected to GC analysis process.

[GC analysis condition]

Detector: micro-cell electron capture detector ( ⁶³ Ni)

Column: HP-5 (30m × 0.25mm i.d., 0.25㎛ film thickness, USA)

Injector: 250 ℃, Detector: 320 ℃, column HP-5, Injection volume: 1µl with the same GC as above, the oven temperature was maintained at 100 ℃ for 2 min, and then heated up to 180 ℃ by 10 ℃ per minute. Then, after holding for 2 minutes, the temperature was raised to 280 ℃ by 5 ℃ per minute, and then maintained for 5 minutes to take 37 minutes.

[GC analysis process]

The solution extracted with ASE is concentrated, dissolved in acetone, put into a vial, and analyzed by GC. The solution injected into the inlet passes through the column, and the decancin and decusinol are separated from the domestic and imported acid detected by the detector. Each chromatogram is shown in the following Table 9,10.

Table 9 shows that the specific components of the domestic donkeys are detected in 30.141 and 31.108 components of decusin and decusinol.

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④ Verification result

Origin identification method of the Angelica tang according to the practice of the present invention

100g per sample, crushed into 50 mesh, and 2g is extracted into a cell for extraction (33ml), one cellulose filter, 2g of sea sand, 4g of chem tube hydromatrix, 2g of sample, 4g of chem tube hydromatrix, 2 g of sea sand were filled in order, mounted on ASE and extracted under conditions of 1 minute preheating, 5 minutes of heating, 5 minutes of settling time, solvent flush% 60,

The solution of each extracted sample is concentrated, dissolved in acetone, placed in a vial, analyzed by GC, and when decursin and decursinol are detected in 30 minutes, it is determined as domestic.

On the other hand, the optimum extraction conditions by accelerated solvent extraction (ASE) was found that the temperature is 80 ℃, pressure 1500psi, the solvent is n-Hexane is the best.

In addition, the analysis conditions of the GC is Injector: 250 ℃, Deterector: 320 ℃, column HP-5, Injection volume: 1 ㎕, the oven temperature (Temperature) is maintained at 100 ℃ for 2 min, 10 ℃ per minute 180 ℃ After the temperature was raised to 2 minutes, and then maintained at 5 ℃ per minute to 280 ℃, it was found that it takes 37 minutes to maintain for 5 minutes.

The identification method of origin by the above method can be used as a method of verifying the origin of other medicines by accurate analysis from the abstract method by visual identification.

Claims (3)

100g per sample, crushed with 50 mesh and sampled 2g, 1 cellulose filter, 2g sea sand, 4g chem tube hydromatrix, 2g sample, chem tube hydromatrix in extraction cell (33ml) 4 g), 2 g of sea sand were filled in this order, mounted in ASE, extracted under conditions of 1 minute preheating, 5 minutes of heating, 5 minutes of settling time, solvent flush% 60, The solution of the extracted sample was concentrated, dissolved in acetone, put into a vial, analyzed by GC, and when decursin and decursinol were detected in 30 minutes, it was determined to be domestic. Characteristic method of identifying Dongguk origin. The method of claim 1, wherein the optimum extraction condition by accelerated solvent extraction (ASE) is a temperature of 80 ℃, pressure 1500psi, the solvent is n-Hexane. According to claim 1, Analysis conditions of GC is Injector: 250 ℃, Deterector: 320 ℃, column HP-5, Injection volume: 1㎛, Oven temperature (Temperature) is maintained at 100 ℃ for 2 min, 10 ℃ per minute After the temperature was raised to 180 ° C. for 2 min, the temperature was raised to 280 ° C. per 5 ° C. per minute, and then maintained for 5 min for 37 min.

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