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Characteristic spectrum identification method for carbonized sanguisorba root formula granules

A technology of formula granule and characteristic map, which is applied in measuring devices, instruments, scientific instruments, etc., to achieve the effects of high precision, good stability and simple method

Inactive Publication Date: 2021-05-07
SICHUAN NEO GREEN PHARMA TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is almost no research on the fingerprints of Burnet charcoal medicinal materials, and the research literature on the formula granules of Burnet charcoal is only TLC identification and HPLC content determination, etc.

Method used

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  • Characteristic spectrum identification method for carbonized sanguisorba root formula granules
  • Characteristic spectrum identification method for carbonized sanguisorba root formula granules
  • Characteristic spectrum identification method for carbonized sanguisorba root formula granules

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0053]Preparation of reference solution Take 0.5g of Burnet reference medicinal material (batch number: 121286-201703), put it in a stoppered Erlenmeyer flask, add 50mL of water, ultrasonicate for 30 minutes, let cool to room temperature, shake well, filter, and take continued The filtrate was used as the reference substance solution of the contrast medicinal material. Take another appropriate amount of ellagic acid reference substance, weigh it accurately, put it in a brown measuring bottle, add 70% methanol to make a solution containing 30μg per 1mL.

[0054] Preparation of the test solution: Take 0.1 g of this product (batch number: GR-DYT-01), accurately weigh it, place it in a stoppered Erlenmeyer flask, add 50 mL of water accurately, weigh it, and ultrasonically process it (power 600W, frequency 40kHz ) for 30 minutes, let cool to room temperature, weigh again, make up for the lost weight with water, shake well, filter, and take the filtrate to obtain the final product. ...

Embodiment 1

[0134] In summary, the RSD of the relative retention time of each characteristic peak meets the requirements in the above investigations, and the method is good. The above nine characteristic peaks were included in the follow-up investigation.

[0135] Verification results of 3 batches of Burnet charcoal formula granules

[0136] The proposed method was used to measure the characteristic spectra of 3 batches of samples of this product, and calculate the relative retention time and relative peak area. Such as Figure 14 , Table 14 and Table 15.

[0137] Table 14 Relative retention time of 3 batches of Burnet charcoal formula granules

[0138]

[0139] Table 15 Relative peak areas of three batches of Burnet charcoal formulation particles

[0140]

[0141] According to the principles of stable relative retention time and relatively high peaks that can be detected in all batches of samples, a total of 9 peaks with good repeatability were selected as characteristic peaks....

Embodiment 2

[0143] Establishment of Specified Value Limits for Relative Retention Time

[0144] See Table 16 and Table 17 for a summary of the methodological inspection items and verification results:

[0145] Table 16 Summary standard of RSD% of each project result of methodology—relative retention time

[0146]

[0147] Table 17 Summary standard of RSD% of methodological project results—relative peak area

[0148]

[0149] It can be seen from the above table that the flow rate has the greatest influence on the relative retention time of the characteristic peaks, so the flow rate is set at 1mL / min. In order to increase the reproducibility and applicability of the method, the relative retention time of each peak is tentatively set at 8%. .

[0150] Final regulation: there should be 9 characteristic peaks in the characteristic spectrum of the test product, among which the peak corresponding to the ellagic acid reference substance is the S peak, and the relative retention time of ea...

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Abstract

The invention discloses a characteristic spectrum identification method for a carbonized sanguisorba root formula granule. The method comprises the following steps: taking 0.5 g of the carbonized sanguisorba root formula granule, adding a test sample extraction solvent, weighing, extracting, cooling, re-weighing, supplementing the lost weight with the test sample extraction solvent, uniformly shaking, filtering, and taking a continuous filtrate; taking a proper amount of ellagic acid, gallic acid and 5-hydroxymethylfurfural reference substances, precisely weighing the reference substances, placing the reference substances in a brown measuring flask, and adding 70% methanol as a reference substance solution of the reference substances; carrying out gradient elution under the following chromatographic conditions: octadecylsilane chemically bonded silica is used as a filler, the column length is 250 mm, the inner diameter is 4.6 mm, and the particle size of silica gel is 5 [mu]m; the detection wavelength of the diode array detector ranges from 220 nm to 360 nm; the column temperature is 20-30 DEG C; the flow velocity is 0.8 to 1.2 mL / min; and a mobile phase A is methanol, and a mobile phase B is a 0.1% phosphoric acid / water mixed solution; and precisely sucking 10 [mu]L of the reference solution and 10 [mu]L of the test solution respectively, injecting the solutions into a liquid chromatograph, and determining to obtain the target product.

Description

technical field [0001] The invention belongs to the technical field of detection of traditional Chinese medicines, and in particular relates to a method for identifying characteristic spectrum of burnet charcoal formula granules. Background technique [0002] Burnet is the dry root of Burnet or Longleaf Burnet, a plant in the Rosaceae family. The latter is commonly known as "cotton elm". Excavate in spring when the plants germinate or wither in autumn, remove fibrous roots, wash and dry, or slice and dry while fresh. Burnet charcoal: Take clean Burnet slices and put them in a pot, heat them with strong fire, fry until the surface is burnt black and the inside is brown, spray a little water to extinguish the sparks, take it out and cool thoroughly. At present, there is almost no research on the fingerprints of Burnet charcoal medicinal materials, and the research literature on the formula granules of Sangui charcoal is only TLC identification and HPLC content determination....

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06Y02A50/30
Inventor 周厚成胡昌江费文波付林高锐周维
Owner SICHUAN NEO GREEN PHARMA TECH DEV