CN-122017070-A - Construction of asparagus and asparagus formulation granules and other asparagus formulation quality control methods

Abstract

The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to construction of asparagus and asparagus formula granules and other asparagus preparation quality control methods. The method comprises the steps of preparing a sample solution, preparing a reference substance solution, detecting by adopting an ultra-high performance liquid chromatography, wherein the conditions comprise a chromatographic column taking octadecylsilane chemically bonded silica as a filler, carrying out gradient elution by taking acetonitrile as a mobile phase A and 0.1% phosphoric acid solution as a mobile phase B, wherein the gradient elution comprises the steps of 0-4 min,1% -6% A,99% -94% B, 4-7 min,6% -11%, 94% -89% B, 7-12 min,11% -15% and 89% -85% B, and constructing a characteristic map and a reference map of radix asparagi or a preparation thereof, and comparing. The quality control method can efficiently determine 8 common peaks of the radix asparagi or the preparation thereof within 12min, identify 3 characteristic peaks, and realize rapid, environment-friendly and comprehensive quality control of radix asparagi medicinal materials, decoction and formula particles.

Inventors

• ZHOU YONGKANG
• LI RUI
• GAO YANG

Assignees

• 北京康仁堂药业有限公司

Dates

Publication Date

20260512

Application Date

20260213

Claims (10)

1. 1. The construction of the quality control method of the asparagus and asparagus prescription granule and other asparagus preparation is characterized by comprising the following steps: (1) Preparing a sample solution, namely dissolving 0.2-1 g of the sample in 5-20 mL of 10% methanol, taking out after ultrasonic treatment, cooling, shaking uniformly, and filtering to obtain the sample solution; (2) Preparing a reference substance solution; (3) Detection is carried out by adopting ultra-high performance liquid chromatography, wherein the conditions of the ultra-high performance liquid chromatography comprise: the chromatographic column takes octadecylsilane chemically bonded silica as a filler, acetonitrile as a mobile phase A and 0.1 percent phosphoric acid solution as a mobile phase B are subjected to gradient elution, wherein the gradient elution process comprises 0-4 min,1% -6% A,99% -94% B, 4-7 min,6% -11%, 94% -89% B, 7-12 min,11% -15% and 89% -85% B; (4) And (3) constructing a characteristic map and a control map of the asparagus or the preparation thereof, and comparing.
2. 2. The method according to claim 1, wherein the ultrasonic treatment in step (1) is performed for 20-40 min, at a power of 200-250W and at a frequency of 40-50 kHz.
3. 3. The method according to claim 1, wherein the step (1) is performed by using a microporous filter membrane, and the pore size of the microporous filter membrane is 0.22-0.45 μm.
4. 4. The method for controlling the quality of asparagus and asparagus formulation granules and other asparagus formulation according to claim 1, wherein the preparation method of the reference solution in step (2) is that tyrosine, phenylalanine and tryptophan standard substances are precisely weighed, and 10% methanol is respectively added to prepare a solution containing 10 mug of standard substances per 1 mL, namely the reference solution.
5. 5. The method according to claim 1, wherein the chromatographic column in step (3) has a column length of 150 mm, an inner diameter of 2.1 to mm and a particle size of 1.8 μm.
6. 6. The construction of the quality control method of asparagus and asparagus formulation particles and other asparagus formulations according to claim 1, wherein the conditions of the ultra performance liquid chromatography in step (3) further comprise: 1) The column temperature is 33-37 ℃; 2) The flow rate is 0.38-0.42 mL/min; 3) The detection wavelength is 201-205 nm; 4) The sample injection amount is 1-2 mu L; 5) The theoretical plate number should be not less than 70000 in terms of phenylalanine peak.
7. 7. The construction of the quality control method of asparagus and asparagus formulation particles and other asparagus formulations according to claim 1, wherein the test substance comprises asparagus medicinal material, asparagus formulation particles or asparagus standard decoction lyophilized powder.
8. 8. The method according to claim 1, wherein the profile comprises 8 common peaks, wherein peak 4 is a reference peak, peak 2 is tyrosine, peak 4 is phenylalanine, and peak 7 is tryptophan.
9. 9. The method according to claim 8, wherein the 8 common peaks have a relative retention time within ±10% of a predetermined value, each of which is defined as peak 1:0.43, peak 2:0.52, peak 3:0.65, peak 4:1.00, peak 5:1.18, peak 6:1.27, peak 7:1.43, and peak 8:1.58, respectively.
10. 10. Use of the granule formulation of asparagus and asparagus formulation according to any of claims 1 to 9 in the construction of a method for quality control of asparagus and formulations thereof.

Description

Construction of asparagus and asparagus formulation granules and other asparagus formulation quality control methods Technical Field The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to construction of asparagus and asparagus formula granules and other asparagus preparation quality control methods. Background Radix asparagi is root tuber of Asparagus cochinchinensis (Asparagus cochinchinensis (Lour.) Merr.) belonging to Liliaceae, has effects of nourishing yin, promoting salivation, moistening lung, clearing heart fire, and is used for treating dry cough due to lung dryness, dry throat, thirst, and internal heat diabetes, and especially has unique advantage in dryness-heat cough. The amino acid in radix asparagi is the main active ingredient, and in addition, saponins. The amino acid component is one of the core substance bases of radix asparagi for playing the traditional effects (nourishing yin, moisturizing dryness, promoting the production of body fluid, quenching thirst and the like), has hydrophilicity, can stimulate salivary glands and sweat glands to secrete, relieve xerostomia, sore throat and xerodermia (such as diabetes dry mouth and climacteric hectic fever and night sweat) caused by yin deficiency and fire excess or body fluid consumption, can promote gastric juice and intestinal juice secretion, improve digestive enzyme activity, relieve yin deficiency constipation (such as senile constipation and postpartum constipation) and reduce discomfort caused by intestinal mucosa dryness. Therefore, it is particularly necessary to control the amino acid content of asparagus. At present, under the asparagus item in Chinese pharmacopoeia (2025 edition), no amino acid related characteristic spectrum test item exists, and only the quality of products is controlled by the test items such as thin layer identification, moisture, extract and the like, so that the quality control is too one-sided, the clinical curative effect of the products is difficult to ensure, and therefore, the integrity of the products is required to be controlled. Although the provincial standard (quality standard of Shanghai Chinese medicine formula granule-radix asparagi; quality standard of Beijing Chinese medicine formula granule-radix asparagi) establishes the radix asparagi characteristic spectrum, the method aims at the saponin component or the aspartic acid hydrolysate of radix asparagi, the method still lacks the whole control of amino acid components, and the detection method is too long (more than 30 minutes), so that the method is difficult to adapt to the high-efficiency and batch detection in the industrial production of the Chinese medicine. In addition, the current literature research on liquid phase detection of radix asparagi is mostly based on saponin components of radix asparagi medicinal materials, and other process steps are not involved basically, so that the method is not necessarily suitable for quality detection of radix asparagi related preparations, the content of the saponin components in radix asparagi is extremely low, the peak number is limited, the efficacy related components are few, the amino acid components are more, the peak number is more, the information amount is large, the components are relatively stable, and the influence of the process is small, so that the amino acid is more suitable for quality detection of radix asparagi different preparations relative to the saponin components. Traditional Chinese medicine is mainly decoction, and amino acid components in the asparagus standard decoction are one of important material bases of curative effects. Therefore, the quality control method using the amino acid as an index is established, the method is more in line with the clinical medication characteristics, and the effectiveness of the method is guaranteed. The traditional Chinese medicine formula granule is a novel formula medicine prepared by taking traditional Chinese medicine decoction pieces as raw materials under the guidance of the theory of traditional Chinese medicine through the processes of extraction, concentration, drying, granulation and the like, and has the advantages of convenience in administration, easiness in carrying, controllable quality and the like. However, as the asparagus formula particles lose the characteristic identification characteristic of decoction pieces, the establishment of a comprehensive and rapid quality detection method of the asparagus formula particles has important significance for realizing the overall quality control. Disclosure of Invention Technical problem In order to solve the problems, the invention provides a quality control method suitable for radix asparagi and a preparation thereof, which strengthens the specificity identification and multi-component and overall quality control according to the characteristics of radix asparagi and the preparation thereof (such as radix asparagi f