Detection and quality control method of tortoise shell, vinegar tortoise shell and formula granules thereof

A detection method and technology of formula particles, which are applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of high cost, complicated preparation and unenvironmental protection, and achieve the effects of stable method, simple processing conditions and high precision.

Active Publication Date: 2022-05-13
BEIJING KANGRENTANG PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Therefore, the problem solved by the present invention is, in the high performance liquid chromatography of existing detection tortoise shell, vinegar tortoise shell and formula particle thereof, the preparation of need testing solution is complicated , high cost, and non-environmental protection, the present invention provides a detection method that can effectively detect tortoise shells, vinegar tortoise shells and their formula particles without acid hydrolysis and derivative reagents

Method used

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  • Detection and quality control method of tortoise shell, vinegar tortoise shell and formula granules thereof
  • Detection and quality control method of tortoise shell, vinegar tortoise shell and formula granules thereof
  • Detection and quality control method of tortoise shell, vinegar tortoise shell and formula granules thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for detecting tortoise shell and vinegar tortoise shell and its formula particles, comprising:

[0043] Obtain the test substance and prepare it into a test solution, wherein the test substance includes three batches of tortoise shell formula granules and a batch of vinegar tortoise shell formula granules; the preparation process of the test solution is: take about 0.5g of formula granules, and Weigh, place in a stoppered Erlenmeyer flask, add 25ml of water precisely, seal the plug, weigh, ultrasonically treat (power 250W, frequency 40kHz) for 30 minutes, let cool, weigh again, make up the lost weight with water, Shake well, filter, and take the filtrate to obtain the test solution of tortoise shell and vinegar tortoise shell formula granules.

[0044] A reference substance solution is prepared, and the reference substance solution includes a contrast medicinal material solution and a contrast substance solution. Wherein, the preparation process of the referen...

Embodiment 2

[0051] A method for detecting tortoise shell and vinegar tortoise shell and formula particles thereof, the difference from Example 1 is that the chromatographic conditions are different, and the specific settings are as follows:

[0052] 1. Detection of different column temperatures

[0053] In this example, 29°C, 30°C, and 31°C were used respectively, and the method of Example 1 was used to detect the characteristic spectrum of the test solution of the tortoiseshell formula granule, and the detection results are shown in Table 2 below.

[0054] Table 2 Relative retention time table at different column temperatures

[0055]

[0056] Summary: It can be seen from the above data that, taking the relative retention time of the characteristic spectrum obtained at 30°C as a reference, the relative retention time of the 6 peaks of the characteristic spectrum obtained at the other two temperatures differs by ±10% from their relative retention time. It has good tolerance to the col...

Embodiment 3

[0078] This embodiment is used to verify the precision and stability of the detection method of a kind of tortoise shell described in Example 1 and vinegar tortoise shell and formula granule thereof, specifically as follows:

[0079] 1. Precision

[0080] 1.1. Repeatability

[0081] Take 6 parts of Guijia formula granules (batch number: 19011411), measure according to the method described in Example 1, obtain its characteristic spectrum, and use peak No. 6 as a reference peak, calculate its relative peak area and relative retention time. And calculate the RSD. The results are shown in Table 6 and Table 7.

[0082] Table 6 Retention time and relative retention time table of characteristic map repeatability investigation

[0083]

[0084]

[0085] Table 7 Characteristic spectrum repeatability investigation peak area and relative peak area

[0086]

[0087] Summary: According to the repeatability investigation results, the relative retention time RSD of each characte...

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Abstract

The invention provides a tortoise shell, a vinegar tortoise shell and a detection and quality control method of formula granules of the tortoise shell and the vinegar tortoise shell. The detection method provided by the invention comprises the following steps: obtaining a test solution of an object to be detected, and the preparation method of the test solution comprises the following steps: obtaining the object to be detected, precisely weighing, adding a solvent, sealing a plug, weighing the weight, carrying out ultrasonic treatment, cooling, re-weighing the weight, complementing the lost weight by using a corresponding solvent, uniformly shaking, filtering, and taking a subsequent filtrate to obtain the test solution; directly performing high performance liquid chromatography detection on the test solution to obtain a characteristic spectrum; in the high performance liquid chromatography detection, methanol is used as a mobile phase A, and a 0.08-0.12% phosphoric acid aqueous solution is used as a mobile phase B. The invention solves the problems of complex preparation, high cost and non-environmental protection of a test solution in the existing high performance liquid chromatography for detecting the tortoise shell, the vinegar tortoise shell and formula granules of the tortoise shell and the vinegar tortoise shell; the rapid and simple detection of the tortoise shells, the vinegar tortoise shells and the formula granules thereof can be effectively realized under the condition of not needing acidolysis and derivatization reagents.

Description

technical field [0001] The invention relates to the field of traditional Chinese medicine detection, in particular to a method for detection and quality control of tortoise shells, vinegar tortoise shells and their formula particles. Background technique [0002] The tortoise shell is the carapace and plastron of the turtle Chinemys reevesii (Gray). It has the effects of nourishing yin and suppressing yang, nourishing kidney and strengthening bones, nourishing blood and nourishing the heart, consolidating meridians and stopping collapse. Metrorrhagia and metrorrhagia. According to textual research, tortoise shell was first recorded in "Shen Nong's Materia Medica", listed as top grade, and is a commonly used traditional Chinese medicine in Chinese medicine. Vinegar tortoise shell is a processed product of tortoise shell. The functions and indications of the two are the same, but the effect of nourishing yin is enhanced after vinegar is made, and it can correct odor and flav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/06G01N30/34
CPCG01N30/8631G01N30/8686G01N30/06G01N30/34
Inventor 张志强安琪史国华吉艳慧张建辉蔡金玲董晨虹
Owner BEIJING KANGRENTANG PHARMA
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