Apocynum venetum leaf formula granule characteristic spectrum identification method

A technology of characteristic maps and formula granules, which is applied in the field of identification of characteristic maps of Apocynum leaf formula granules, can solve the problems of lack, difficulty in quality monitoring of Apocynum leaf formula granules, etc., achieve high precision, simple method, and ensure the effect of drug safety

Active Publication Date: 2021-04-30
SICHUAN NEO GREEN PHARMA TECH DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is a lack of qualitative research literature on Apocynum leaf formula granules, and it is difficult to monitor the quality of Apocynum leaf formula granules

Method used

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  • Apocynum venetum leaf formula granule characteristic spectrum identification method
  • Apocynum venetum leaf formula granule characteristic spectrum identification method
  • Apocynum venetum leaf formula granule characteristic spectrum identification method

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Experimental program
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Effect test

preparation example Construction

[0060] Preparation of reference substance solution Take hyperoside, caffeic acid, chlorogenic acid, astragalin, neochlorogenic acid, cryptochlorogenic acid, isoquercitrin reference substance amount, accurately weighed, add 70% methanol to make Each 1mL containing 30μg of the solution, that is.

[0061] Preparation of reference medicinal material solution Take 0.5 g of apocynum leaf reference medicinal material, accurately weigh, put in a stoppered Erlenmeyer flask, accurately add 50 mL of 70% methanol, seal tightly, weigh, and ultrasonically process (power 600W, frequency 40kHz) for 20 Minutes, let cool, weigh again, make up for the lost weight with 70% methanol, shake well, filter, and take the filtrate to obtain the final product.

[0062] Preparation of the test solution Take this product under the difference in loading amount, mix it evenly, take an appropriate amount, grind it finely, get 0.25g of Apocynum leaf formula granules, accurately weigh it, put it in a stoppered ...

Embodiment 1

[0148] Verification results of 3 batches of Apocynum leaf formula granules

[0149] 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 17 , Table 15 and Table 16.

[0150] Table 6 Relative retention time of 3 batches of Apocynum leaf formula granules

[0151]

[0152] Table 7 Relative peak areas of 3 batches of Apocynum leaf formula granules

[0153]

[0154] According to the principle of stable relative retention time and the detection of each batch of samples with relatively high peaks, a total of 7 peaks with good repeatability were selected as characteristic peaks. The results showed that when peak 5 was used as the S peak, the relative retention time RSDs of the characteristic peaks of the 3 batches of Apocynum leaf formula granules were between 0.01% and 0.06%, and the relative retention time RSDs of the 7 characteristic peak...

Embodiment 2

[0156] Establishment of Specified Value Limits for Relative Retention Time

[0157] See Table 17 and Table 18 for a summary of the methodological inspection items and verification results:

[0158] Table 8 Summary standard of RSD% of methodological project results—relative retention time

[0159]

[0160]

[0161] Table 18 Summary standard of RSD% of methodological project results—relative peak area

[0162]

[0163] It can be seen from the above table that the flow rate has the greatest influence on each characteristic peak, so the flow rate is set at 1mL / min, referring to the results of instrument and chromatographic column durability, in order to increase the reproducibility and applicability of the method, the relative retention time of each peak The specified value is tentatively set at 8%; and the durability and verification results have a great influence on the relative peak area, so the relative peak area is not included in the standard.

[0164] Final regul...

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Abstract

The invention discloses an apocynum venetum leaf formula granule characteristic spectrum identification method which comprises the following steps: taking 0.25 g of apocynum venetum leaf formula granule, precisely weighing, placing into a conical flask with a plug, precisely adding an extraction solvent, extracting for 10-30 min, cooling, uniformly shaking, filtering, and taking the subsequent filtrate; taking a proper amount of hyperoside, caffeic acid, chlorogenic acid, astragalus smicus glycoside, neochlorogenic acid, cryptochlorogenic acid and isoquercitrin reference substances, and adding 70% methanol to prepare a solution; 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 is 220-360nm; the column temperature is 20-30 DEG C; the flow rate is 0.8-1.2 mL / min; mobile phase: acetonitrile is used as a mobile phase A, a 0.2% phosphoric acid solution is used as a mobile phase B, and gradient elution is carried out; precisely sucking 10 microliters of the reference solution, 10 microliters of the reference medicinal material solution and 10 microliters of the test solution respectively, injecting into a liquid chromatograph, and measuring.

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 a feature spectrum of apocynum leaf formula granules. Background technique [0002] Apocynum erect semi-shrub, 1.5-3 meters high, generally about 2 meters high, up to 4 meters high; branches opposite or alternate, cylindrical, smooth and hairless, purple or light red. Leaves opposite, subopposite only at branches, leaves elliptic-lanceolate to oval-oblong, 1-5 cm long, 0.5-1.5 cm wide, apex acute to blunt, with short pointed , base acute to blunt, leaf margin with thin teeth, both sides glabrous; leaf veins slender, slightly convex or flat on the back of the leaf, not obvious on the leaf surface, 10-15 lateral veins on each side, reticulated in front of the leaf margin; Petiole 3-6 mm long; glands between petioles, shedding when old. Apocynum leaves, the name of Chinese medicinal materials. This product is...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
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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