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Method for detecting asarum medicinal material by combining air current purging micro syringe extraction technique with GC-MS (gas chromatography-mass spectrometer)

A GC-MS and micro-injector technology, which is applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of unfavorable identification of the authenticity of Asarum

Inactive Publication Date: 2012-09-26
YANBIAN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

In the Chinese Pharmacopoeia, the method of determining the content of volatile oil and the method of determining the content of asarin in the Chinese Pharmacopoeia are used for quantitative analysis. However, other plants also contain asarin compounds. Disadvantage of identification
Therefore, only the determination of the content of asarin can not fully reflect the whole picture of Asarum medicinal material

Method used

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  • Method for detecting asarum medicinal material by combining air current purging micro syringe extraction technique with GC-MS (gas chromatography-mass spectrometer)
  • Method for detecting asarum medicinal material by combining air current purging micro syringe extraction technique with GC-MS (gas chromatography-mass spectrometer)
  • Method for detecting asarum medicinal material by combining air current purging micro syringe extraction technique with GC-MS (gas chromatography-mass spectrometer)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. The source of medicinal materials Jilin

[0028] 2. Sample number 20110921

[0029] 3. Preparation and detection of the test solution

[0030] The first step: ① Preparation of the test solution

[0031] Accurately weigh 20 mg of the identified Herba Asarum powder (through a 100-mesh sieve), put it in the sample tank, add 20 μL of n-hexane into a 250 μL micro-syringe for extraction, the extraction temperature is 250 ° C, and the extraction time is 2 min, the condensation temperature was -4°C, and the nitrogen flow rate was 2 mL / min. After the extraction, dilute to 100 μL with n-hexane and set aside.

[0032] ② Chromatographic conditions

[0033] Chromatographic column DB-5MS quartz capillary column (30 m × 0.25 mm × 0.25 μm);

[0034] Injection port temperature: 280°C;

[0035] MS detector temperature: 200°C,

[0036] Injection volume: 2 μL,

[0037] Gas phase and mass spectrometer connection port temperature: 280°C;

[0038] Heating program: the initial temp...

Embodiment 2

[0054] Example 2 Detection of Herba Asarum Medicinal Material

[0055] 1. Source of medicinal materials Liaoning

[0056] 2. Sample number 20110926

[0057] 3, prepare need testing solution with the same method of above-mentioned embodiment 1

[0058] 4, measure need testing solution with the same method of above-mentioned embodiment 1

[0059] 5. Result judgment

[0060] In the chromatogram, 23 characteristic peaks that were the same as those of the control fingerprint of Herba Asarum were detected; the fingerprints of the test product and the fingerprint of Herba Asari had a common pattern, which was calculated by the computer-aided similarity evaluation system, and the correlation coefficient was 0.96 , greater than 0.90. Therefore, it can be judged that this test product meets the quality standard about the Asarum medicinal material revised by the present invention.

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Abstract

The invention relates to a method for detecting asarum medicinal material by combining an air current purging micro syringe extraction technique with a GC-MS (gas chromatography-mass spectrometer). The method comprises the following steps of: (1) preparing asarum sample solution; (2) providing chromatographic conditions; (3) creating an asarum medicinal material fingerprint common model map; and (4) controlling quality of the fingerprint; comparing the obtained sample fingerprint with a contrast fingerprint, and inputting the obtained sample fingerprint and the contrast fingerprint into a computer-assisted similarity evaluation system to calculate similarity, so as to obtain a correlation coefficient, thus reaching a detection conclusion. The method disclosed by the invention has the following characteristics: (1) quality of the asarum medicinal material can be generally and macroscopically represented; (2) good specificity and reproducibility can be obtained; operability is strong; and (3) the method disclosed by the invention can be used for identifying the authenticity of the asarum medicinal material.

Description

technical field [0001] The invention belongs to a detection method of traditional Chinese medicinal materials, and specifically refers to a method for detecting the medicinal materials of Asarum chinensis by combining an airflow purging micro-syringe extraction technology and GC-MS. Background technique [0002] Asarum is derived from the dried roots and rhizomes of Asarum heterotropoides Fr. Schmidt val. Mandshuricum (Maxim.) Kitag., a plant of the Aristolochiaceae family, which is recorded in the Chinese Pharmacopoeia. The whole herb of Asarum contains 1%~3% of volatile oil, and the ones with higher content are safrole, 3,5-dimethoxytoluene, elemin, carvone, pinene, imitative pinene, and asarone and other ingredients. In the Chinese Pharmacopoeia, the method of determining the content of volatile oil and the method of determining the content of asarin by high-performance liquid phase are used for quantitative analysis. However, other plants also contain asarin compounds, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 李东浩张善玉朴相范杨翠
Owner YANBIAN UNIV