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Method for identifying characteristic chromatogram of sargentgloryvine stem formula granule

A technology of formula granules and characteristic maps, applied in instruments, measuring devices, scientific instruments, etc., to achieve the effect of ensuring drug safety, good stability, and high precision

Active Publication Date: 2021-05-07
SICHUAN NEO GREEN PHARMA TECH DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The literature review also only found that there were studies on the relevant quality standards of compound Daxueteng granules with salidroside as the index component, and there was no research on single-species Daxueteng formula granules.

Method used

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  • Method for identifying characteristic chromatogram of sargentgloryvine stem formula granule
  • Method for identifying characteristic chromatogram of sargentgloryvine stem formula granule
  • Method for identifying characteristic chromatogram of sargentgloryvine stem formula granule

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[0053]Preparation of Reference Substance Solution Take 1.5g of Rhizoma sagittata reference medicinal material, accurately weigh it, put it in a stoppered Erlenmeyer flask, accurately add 50mL of water, weigh it, heat to 92-98°C for 30 minutes, let cool, and water Make up for the lost weight, filter, evaporate the filtrate to dryness, precisely add 25mL of 50% methanol to the residue, seal it up, ultrasonicate (power 600W, frequency 40kHz) for 30 minutes, let cool, shake well, filter, take the subsequent filtrate as Control medicinal material reference substance solution. Take another appropriate amount of chlorogenic acid reference substance, weigh it accurately, add 50% methanol to make a solution containing 50 μg per 1 mL, and use it as the reference substance solution of the reference substance.

[0054] Preparation of the test solution Take an appropriate amount of this product, grind it finely, get about 0.5g, accurately weigh it, put it in a stoppered Erlenmeyer flask, a...

Embodiment 1

[0137] 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 six characteristic peaks were included in the follow-up investigation.

[0138] Verification results of 3 batches of Daxueteng formula granules

[0139] 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. like Figure 15 , Table 15 and Table 16.

[0140] Table 15 Relative retention time of 3 batches of Daxueteng formula granules

[0141]

[0142] Table 16 Relative peak area of ​​3 batches of Daxueteng formula granules

[0143]

[0144] According to the principle of stable relative retention time and the detection of each batch of samples with relatively high peaks, a total of 6 peaks with good repeatability were selected as characteristic peaks. The results showed that when the...

Embodiment 2

[0146] Establishment of Specified Value Limits for Relative Retention Time

[0147] See Table 17 for a summary of the methodological inspection items and verification results:

[0148] Table 17 Summary standard of RSD% of methodological project results—relative retention time

[0149]

[0150]

[0151] It can be seen from the above table that the flow rate, different instruments, and different chromatographic columns have a great influence on the relative retention time of each characteristic peak, so the flow rate is set as 1.0mL / min. In order to increase the reproducibility and applicability of the method, the The specified value of relative retention time is tentatively set at 8%.

[0152] Final regulation: there should be 6 characteristic peaks in the chromatogram of the test product, and should correspond to the retention time of the 6 characteristic peaks in the solution chromatogram of the reference medicinal material, and the peak corresponding to the chlorogeni...

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Abstract

The invention discloses a method for identifying the characteristic chromatogram of a sargentgloryvine stem formula granule. The method comprises the following steps: taking 0.5 g of the sargentgloryvine stem formula granule, adding a test sample extraction solvent, weighing, extracting, cooling, weighing again, complementing the reduced weight by using the test sample extraction solvent, uniformly shaking, filtering, and taking a subsequent filtrate; taking a proper amount of protocatechuic acid, chlorogenic acid, neochlorogenic acid and cryptochlorogenic acid reference substances, precisely weighing, and adding 50% methanol as a reference substance solution of the reference substances; carrying out gradient elution under the following chromatographicconditions: 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; a detector is a diode array detector, and the detection wavelength is 240-360 nm; the column temperature is 20-40 DEG C; the flow velocity is 0.8 to 1.2 mL / min; and mobile phases comprise a mobile phase A of acetonitrile, and a mobile phase B of 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 detecting 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 spectra of Daxueteng formula granules. Background technique [0002] Sargassum is the dry cane of the plant Akebiae Sargentina. Harvest in autumn and winter, remove side branches, cut into sections, and dry. Distributed in the Yellow River Basin, Qinling Mountains and south of China. It has the effects of clearing heat and detoxifying, promoting blood circulation, expelling wind and relieving pain. For intestinal abscess abdominal pain, pyretic sores, amenorrhea, dysmenorrhea, tumbling and swelling pain, rheumatic arthralgia. The traditional Chinese medicine Caulis Spatholobus has various pharmacological activities, but in clinical practice, Caulis Spatholobus is mainly compatible with other Chinese herbal medicines. The literature review also only found that there were studies on the relev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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
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