Content determination method suitable for Zuogui pill production process

Abstract

The invention relates to the technical field of Zuogui pill production, and discloses a content determination method suitable for the Zuogui pill production process, which comprises the following steps: 1, taking about 1.2 g of sample, precisely weighing, and placing in a conical flask with a plug; step 2, precisely adding 25ml of 50% methanol solution into the conical flask in the step 1; 3, the conical flask in the step 2 is put into an ultrasonic device to be subjected to ultrasonic oscillation treatment for 1 hour; 4, taking out the conical flask in the step 3 from the ultrasonic device, cooling, adding a methanol solution into the conical flask to complement the loss weight, and uniformly shaking; and step 5, filtering the solution in the conical flask in the step 4, then pouring 1-2ml of subsequent filtrate into the small sample injection bottle as a solution to be detected, precisely sucking 10 microliters of the solution to be detected, injecting the solution to be detected into a liquid chromatograph, and determining the content. According to the content determination method suitable for the Zuogui pill production process, compared with reflux, ultrasonic treatment has the advantages that energy consumption is reduced, worries about scalding of experimenters are relieved, the number of detection batches is increased through ultrasonic treatment, the detection period is shortened, and the method is simpler and more convenient.

Description

Technical Field

[0001] The invention relates to the technical field of Zuogui Pill production, and in particular to a content determination method suitable for the Zuogui Pill production process. Background Art

[0002] Zuogui Pills come from Volume 51 of Jingyue Complete Works by Zhang Jingyue, a famous doctor in the Ming Dynasty. It is based on the famous Yin-tonifying prescription "Liuwei Dihuang Pill" with additions and subtractions. It is mainly used to treat dizziness, soreness of the waist and knees, spermatorrhea, spontaneous sweating and night sweats caused by kidney yin deficiency. In recent years, it has been often used to treat senile chronic bronchitis, hypertension, senile dementia, chronic nephritis, lumbar muscle strain, infertility and other patients with true yin deficiency. At the same time, it is also used to treat functional uterine bleeding in women (mainly for patients with kidney yin deficiency and yin and yang deficiency), as well as symptoms such as dizziness and tinnitus caused by liver and kidney deficiency and insufficient essence and blood. The prescription of Zuogui Pill consists of cooked rehmannia, yam, wolfberry, cornus, dodder seed, antler glue, tortoise shell glue, and Achyranthes bidentata. Cooked rehmannia is the main medicine in the prescription, which nourishes kidney yin; among the minister medicines, yam nourishes the spleen and kidney, cornus officinalis astringes the essence and restrains sweat, and tortoise and deer glues are important kidney-tonifying medicines; wolfberry invigorates the essence and improves eyesight, dodder seed and Achyranthes bidentata strengthen the waist and knees, and strengthen the tendons and bones, all of which are adjuvant medicines. The combination of these medicines is mainly used to treat symptoms such as dizziness, soreness of the waist and knees, spermatorrhea, spontaneous sweating and night sweats caused by insufficient kidney yin. The ingredients of Chinese herbal medicines are relatively complex, and there may be differences between different batches. Therefore, it is necessary to accurately determine their content through scientific methods to ensure their stable quality and reliable efficacy. The introduction of modern analytical techniques such as high performance liquid chromatography (HPLC) has brought unprecedented accuracy and reliability to the content analysis of Zuogui Pills. With its high sensitivity, excellent accuracy and strong reproducibility, modern technology has successfully unlocked the secrets of the complex ingredient system of Zuogui Pills and achieved accurate quantification of multiple active ingredients. With the development of modernization and internationalization of traditional Chinese medicine, the quality control requirements for Chinese medicine preparations are getting higher and higher, and the verification of content analysis methodology has become an important link in ensuring the quality of Chinese medicine preparations.

[0003] The existing determination of the content of Zuogui Pills is generally achieved by heating and reflux, but the heating and reflux method consumes a lot of energy, and the temperature of the water bath is high, which poses a safety hazard and the experimenters are easily scalded. At the same time, the heating and reflux method has a small number of test batches and a long test cycle, which is not simple enough. In view of the above problems, the existing equipment needs to be improved. Summary of the invention

[0004] The purpose of the present invention is to provide a content determination method suitable for the production process of Zuogui Pills, so as to solve the problem that the existing Zuogui Pills content determination proposed in the above background technology is generally achieved by heating reflux, but the heating reflux method has relatively large energy consumption, and the temperature of the water bath is high, there are safety hazards, and the experimenters are easily scalded. At the same time, the heating reflux method has a small number of detection batches, a long detection cycle, and is not simple enough.

[0005] To achieve the above object, the present invention provides the following technical solution: a content determination method suitable for the production process of Zuogui Pills, comprising the following steps:

[0006] Step 1: Take about 1.2 g of sample, weigh accurately, and place in a stoppered conical flask;

[0007] Step 2: Accurately add 25 ml of 50% methanol solution to the conical flask in step 1;

[0008] Step 3: Place the conical flask in step 2 into an ultrasonic device for ultrasonic oscillation treatment;

[0009] Step 4: Take out the conical flask in step 3 from the ultrasonic device, let it cool, add methanol solution to the conical flask to make up for the weight loss, and shake well;

[0010] Step 5: Filter the solution in the conical flask in step 4, then take 1-2 ml of the filtrate and pour it into an injection vial as the test solution. Accurately pipette 10 μl of the test solution and inject it into the liquid chromatograph to determine the content.

[0011] Preferably, in step 3, the ultrasonic treatment time is 1 hour, the temperature is 40-60° C., and the ultrasonic frequency is 53HZ.500W.

[0012] Preferably, the concentration of the methanol solution in step 4 is 50%.

[0013] Compared with the prior art, the present invention has the following beneficial effects:

[0014] This method is applicable to the content determination in the production process of Zuogui Pills. It uses ultrasound. The advantages of ultrasound over reflux are as follows:

[0015] (1) Energy saving: reducing the use of tap water in the laboratory.

[0016] (2) Operational hazards: The water bath has a high temperature, which poses a safety hazard and eliminates the worry of burns to the experimenters.

[0017] (3) Since the production process of Zuogui Pills of our company is continuous, this method is also suitable for the detection of intermediates in the production process. Ultrasonic treatment increases the number of test batches, shortens the test cycle, and is more convenient. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is the content data summary table of Zuogui Pills finished product;

[0019] Figure 2 This is a comparison chart of the heating reflux content and the ultrasonic treatment content data. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technical personnel in this field without creative work are within the scope of protection of the present invention.

[0021] The present invention provides a technical solution: a content determination method applicable to the production process of Zuogui Pills, comprising the following steps:

[0022] Example 1

[0023] Step 1: Take about 1.2 g of sample, weigh accurately, and place in a stoppered conical flask;

[0024] Step 2: Accurately add 25 ml of 50% methanol solution to the conical flask in step 1;

[0025] Step 3: Place the conical flask in step 2 into an ultrasonic device and perform ultrasonic treatment for 1 hour (temperature is 40-60°C) at a frequency of 53 Hz.500 W;

[0026] Step 4: Take out the conical flask in step 3 from the ultrasonic device, let it cool, add 50% methanol solution to the conical flask to make up for the weight loss, and shake well;

[0027] Step 5: Filter the solution in the conical flask in step 4, then take 1-2 ml of the filtrate and pour it into an injection vial as the test solution. Accurately pipette 10 μl of the test solution and inject it into the liquid chromatograph to determine the content (refer to Table 1).

[0028] Example 2

[0029] Step 1: Take about 1.2g of sample and weigh accurately.

[0030] Step 2: Place the sample in a stoppered conical flask, accurately add 25 ml of 50% methanol solution, and weigh the weight;

[0031] Step 3: Heat the sample under reflux for 1 hour, cool, make up the lost weight with 50% methanol solution, shake well, filter and take the filtrate.

[0032] The raw material Cornus officinalis (y2206001) was selected, and 10 batches of the corresponding Zuogui Pills were selected for content detection. The heating reflux and ultrasonic treatment were used for data comparison (reference Figure 1), the total amount of morroniside and loganin was: 2.3-2.5%, with an average of 2.4%. The sample pretreatment method was reflux temperature of 85°C, modified to ultrasound (temperature of 40-60°C), ultrasound frequency of 53HZ.500W, and ultrasound time of 1 hour. It was found that with the increase of temperature, the extraction rates of loganin and morroniside tended to be stable and had no effect.

[0033] The above shows and describes the basic principles, main features and advantages of the present invention. Technical personnel in this industry should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only preferred examples of the present invention and are not used to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.

[0034] The directions or positional relationships indicated by terms such as "center", "longitudinal", "lateral", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" are based on the directions or positional relationships shown in the accompanying drawings. They are merely simplified descriptions for the convenience of describing the present invention, and do not indicate or imply that the devices or elements referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they should not be understood as limitations on the protection content of the present invention.

[0035] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for determining the content of Zuogui Pills in the production process, characterized in that: The following steps are involved: Step 1: Take about 1.2 g of sample, weigh accurately, and place in a stoppered conical flask; Step 2: Accurately add 25 ml of 50% methanol solution to the conical flask in step 1; Step 3: Place the conical flask in step 2 into an ultrasonic device for ultrasonic oscillation treatment; Step 4: Take out the conical flask in step 3 from the ultrasonic device, let it cool, add methanol solution to the conical flask to make up for the weight loss, and shake well; Step 5: Filter the solution in the conical flask in step 4, then take 1-2 ml of the filtrate and pour it into an injection vial as the test solution. Accurately pipette 10 μl of the test solution and inject it into the liquid chromatograph to determine the content.

2. A method for determining the content of Zuogui Pills in the production process according to claim 1, characterized in that: In step 3, the ultrasonic treatment time is 1 hour, the temperature is 40-60° C., and the ultrasonic frequency is 53HZ.500W.

3. A method for determining the content of Zuogui Pills in the production process according to claim 1, characterized in that: The concentration of the methanol solution in step 4 is 50%.

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