Method for detecting fingerprint spectrum of instant zizyphus jujube benoxinning solid beverage

文档序号:1844637 发布日期:2021-11-16 浏览:10次 中文

阅读说明:本技术 速溶酸枣仁心宁饮固体饮料指纹图谱的检测方法 (Method for detecting fingerprint spectrum of instant zizyphus jujube benoxinning solid beverage ) 是由 金俊杰 李国维 刘爱国 于 2021-07-31 设计创作,主要内容包括:本发明公开了速溶酸枣仁心宁饮固体饮料指纹图谱的检测方法,它包括步骤1、供试品溶液的制备;步骤2、混合对照品溶液的制备:步骤3、分别精密吸取混合对照品溶液和供试品溶液注入液相色谱仪,记录色谱图;步骤4,将供试品溶液指纹图谱从仪器导出,导入中药色谱指纹图谱相似度评价系统,选择不同批次速溶酸枣仁心宁饮固体饮料的色谱图中均存在的色谱峰作为共有峰;用平均值计算法生成速溶酸枣仁心宁饮固体饮料的对照指纹图谱;计算各共有峰的相对保留时间、相对峰面积;并与混合标准品图谱进行比对,指认主要成分峰。本发明指纹图谱,能全面,客观地表征速溶酸枣仁心宁饮固体饮料的质量。检测方法简便、稳定、精密度高、重现性好等优点。(The invention discloses a method for detecting a fingerprint spectrum of an instant zizyphus jujube benoxinning solid beverage, which comprises the steps of 1, preparing a test solution; step 2, preparation of a mixed reference solution: step 3, respectively and precisely sucking the mixed reference solution and the test solution to be injected into a liquid chromatograph, and recording a chromatogram; step 4, leading out the fingerprint of the sample solution from the instrument, leading the sample solution into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, and selecting chromatographic peaks existing in the chromatograms of different batches of instant zizyphus jujube renxinning solid beverages as common peaks; generating a comparison fingerprint of the instant zizyphus jujube kernel xinning solid beverage by using an average value calculation method; calculating the relative retention time and the relative peak area of each common peak; and comparing with the mixed standard substance spectrum to identify the main component peak. The fingerprint spectrum of the invention can comprehensively and objectively characterize the quality of the instant zizyphus jujube benoxinning solid beverage. The detection method has the advantages of simplicity, stability, high precision, good reproducibility and the like.)

1. A method for detecting a fingerprint spectrum of an instant zizyphus jujube kernel xinning solid beverage is characterized by comprising the following steps:

step 1, preparing an instant zizyphus jujube benxinning solid beverage test solution:

weighing different batches of instant solid beverage fluid extract samples of Zizyphi Spinosae semen XINNING, adding methanol solution, ultrasonic extracting, centrifuging the extractive solution, collecting supernatant, and filtering with 0.45 μm microporous membrane to obtain test solution;

step 2, preparation of mixed reference solution:

precisely weighing chlorogenic acid, puerarin and formononetin reference substances, placing in a volumetric flask, adding methanol to constant volume to scale, shaking up, and making into mixed reference substance solution;

step 3, precisely absorbing the test solution obtained in the step 1 and the mixed reference solution obtained in the step 2 respectively, injecting the solutions into a high performance liquid chromatograph, and recording a chromatogram;

step 4, exporting the fingerprint of the test solution of the instant zizyphus jujube renxinning solid beverage obtained in the step 3, and importing the fingerprint into a traditional Chinese medicine chromatography fingerprint similarity evaluation system 2012A; selecting chromatographic peaks existing in chromatograms of different batches of instant zizyphus jujube kernel xinning solid beverages as common peaks; generating a comparison fingerprint of the instant zizyphus jujube kernel xinning solid beverage by using an average value calculation method, and calculating the relative retention time and the relative peak area of each common peak; marking chemical components of peaks in the comparison fingerprint spectrum according to the retention time of the mixed reference solution chromatogram;

and 5, comparing the fingerprint spectrum of the instant solid beverage of zizyphus jujube renxinning obtained in the step 3 with the spectrum of the mixed standard substance, and identifying that the No. 8 peak in the instant solid beverage of zizyphus jujube renxinning is chlorogenic acid, the No. 9 peak is puerarin and the No. 26 peak is formononetin.

2. The method for detecting the fingerprint of the instant solid beverage of zizyphus jujube renxinning according to claim 1, wherein the preparation method of the sample solution of the instant solid beverage of zizyphus jujube renxinning in step 1 comprises the following steps: taking 5-10 g of 8 batches of instant zizyphus jujube kernel xinning solid beverage clear paste samples, adding 6-20 times of methanol, placing the mixture into a round bottom flask, carrying out ultrasonic extraction for 1-3 times, 0.5-1 hour each time, centrifuging the extracting solution, and filtering the supernatant with a 0.45 mu m microporous filter membrane to obtain a sample solution.

3. The method for detecting the fingerprint of the instant zizyphus jujube renxinning solid beverage as claimed in claim 1, wherein the step 2 is to prepare a mixed reference solution: precisely weighing chlorogenic acid, puerarin and formononetin as reference substances, placing in a volumetric flask, adding methanol to constant volume to scale, shaking, and making into mixed reference substance solution containing 0.1019mg/mL chlorogenic acid, 0.1008mg/mL puerarin and 0.1022mg/mL formononetin.

4. The method for detecting the fingerprint of the instant zizyphus jujube kernel xinning solid beverage as claimed in claim 1, wherein in the step 3, the liquid chromatography conditions are as follows: a chromatographic column: YMC-Pack ODS-A, mobile phase: acetonitrile and 0.1% phosphoric acid water, gradient elution, diode array detector, detection wavelength: 254nm, column temperature 30 ℃, flow rate 0.9mL/min, sample injection volume: 10 μ L, gradient elution procedure as follows:

5. the method for detecting the fingerprint of the instant zizyphus jujube benoxinning solid beverage according to claim 1, wherein the fingerprint contains 27 peaks, the retention time of which is 10.866min, 12.068min, 12.971min, 15.404min, 16.496min, 17.514min, 19.578min, 25.235min, 28.92min, 30.936min, 9min, 40.996min, 41.843min, 45.584min, 47.114min, 50.515min, 52.265min, 53.458min, 55.378min, 32.156min, 41.843min, 45.584min, 47.114min, 55.378min, 3626 min, and the peak of chlorogenic acid, formononetin, wherein the mangiferin peak 3626 and the mangiferin peak is the peak of Oenanthes No. 1.

6. The method for detecting the fingerprint of the instant solid beverage of the wild jujube kernel xinning as claimed in any one of claims 1 to 5, wherein the instant solid beverage of the wild jujube kernel xinning comprises the following components in parts by weight: 15-30 parts of spina date seed, 10-20 parts of ginseng, 12-24 parts of poria cocos, 7-14 parts of medlar, 5-10 parts of cinnamon, 7-14 parts of kudzu root, 5-10 parts of platycodon grandiflorum, 7-14 parts of Chinese date, 6-12 parts of lotus seed, 6-12 parts of lily, 5-10 parts of cassia seed, 5-10 parts of cape jasmine, 5-10 parts of liquorice and 5-10 parts of hawthorn.

7. The method for detecting the fingerprint of the instant solid beverage of the wild jujube kernel xinning as claimed in claim 6, wherein the instant solid beverage of the wild jujube kernel xinning comprises the following components in parts by weight: 15 parts of spina date seed, 10 parts of ginseng, 12 parts of poria cocos, 7 parts of medlar, 5 parts of cinnamon, 7 parts of radix puerariae, 5 parts of platycodon grandiflorum, 7 parts of Chinese date, 6 parts of lotus seed, 6 parts of lily, 5 parts of cassia seed, 5 parts of gardenia, 5 parts of liquorice and 5 parts of hawthorn.

Technical Field

The invention relates to a detection method of a traditional Chinese medicine instant solid beverage, in particular to a detection method of a fingerprint spectrum of an instant zizyphus jujube benoxinning solid beverage.

Background

Insomnia is the most common sleep disorder in the clinic. The long-term serious insomnia not only can bring negative effects to the body, life, interpersonal relationship and work of the patient, but also can even cause the occurrence of malignant accidents. Under the conditions of insufficient sleep and poor sleep quality for a long time, the problems of mental disorder, memory decline, concentration failure, emotional instability and the like can be caused, and the daily life is further influenced. Even if the immunity is seriously reduced, the human body is easily infected by infectious diseases, or symptoms such as headache, dizziness, melancholy and the like are caused. The instant zizyphus jujube kernel xinning solid beverage is beneficial to conditioning physique and improving insomnia troubles aiming at different types of insomnia patients.

The spina date seed in the formula has the effects of nourishing heart, tonifying liver, calming heart, soothing nerves, promoting fluid production and arresting sweating; the ginseng is sweet and warm, has the effects of tonifying qi and strengthening middle warmer, and enhances the immunity; poria cocos is used for treating insomnia due to spleen deficiency, and promoting diuresis and excreting dampness; the medlar can nourish liver and kidney, benefit essence and improve eyesight; cinnamon has the effects of tonifying fire and supporting yang, dispelling cold and relieving pain, and warming and activating channels and collaterals; radix Puerariae has effects of relieving muscles and fever, dredging meridian passage; the platycodon grandiflorum has the effects of dispersing lung qi, eliminating phlegm and relieving sore throat; the Chinese dates have the effects of tonifying middle-jiao and Qi, nourishing blood and soothing nerves; the lotus seeds can tonify spleen to stop diarrhea, tonify kidney to arrest seminal emission, nourish heart to calm mind; bulbus Lilii has effects in moistening lung, relieving cough, clearing heart fire, and tranquilizing mind; semen Cassiae has effects of relaxing bowels, smoothing intestine, removing liver fire and improving eyesight; cape jasmine fruit cools blood and detoxifies, clears heat and promotes diuresis; the liquorice tonifies spleen and qi, clears away heat and toxic materials, eliminates phlegm and stops coughing, relieves spasm and pain; haw promotes digestion, invigorates stomach, promotes qi circulation, removes blood stasis, eliminates turbid pathogen and reduces blood fat. The ingredients in the formula respectively play their own roles, so that the effects of nourishing heart and soothing nerves are achieved, and the resistance of a human body is enhanced, so that the Chinese medicinal composition can be used for auxiliary dietary therapy of vexation and insomnia.

At present, the quality detection method of the instant zizyphus jujube kernel xinning solid beverage is less. The invention adopts the high performance liquid chromatography to establish the fingerprint detection method of the instant zizyphus jujube kernel xinning solid beverage, and has important significance for ingredient identification, quality evaluation and quality standard formulation of the instant zizyphus jujube kernel xinning solid beverage.

Disclosure of Invention

The purpose of the invention is as follows: the invention aims to solve the defects of the prior art and provides the fingerprint detection method of the instant solid beverage of the zizyphus jujube renxinning, and the detection method can objectively, comprehensively and accurately evaluate the quality of the instant solid beverage of the zizyphus jujube renxinning and has important significance for controlling the quality of the instant solid beverage of the zizyphus jujube renxinning and ensuring the clinical curative effect.

The technical scheme is as follows: in order to achieve the purpose, the invention adopts the technical scheme that:

a method for detecting a fingerprint spectrum of an instant zizyphus jujube kernel xinning solid beverage is characterized by comprising the following steps:

step 1, preparing an instant zizyphus jujube benxinning solid beverage test solution:

accurately weighing different batches of the fluid extract samples of the instant zizyphus jujube renxinning solid beverage, placing the fluid extract samples in a round-bottomed flask, carrying out ultrasonic extraction, centrifuging an extracting solution, and filtering supernate with a 0.45 mu m microporous filter membrane to obtain a test sample solution;

step 2, preparation of mixed reference solution:

precisely weighing chlorogenic acid, puerarin and formononetin reference substances, placing in a volumetric flask, adding methanol to constant volume to scale, shaking up, and making into mixed reference substance solution;

step 3, precisely absorbing the test solution in the step 1 and the reference solution in the step 2 respectively, injecting the test solution and the reference solution into a high performance liquid chromatograph, and recording a chromatogram;

step 4, exporting the fingerprint of the test solution of the instant zizyphus jujube renxinning solid beverage obtained in the step 3, and importing the fingerprint into a traditional Chinese medicine chromatography fingerprint similarity evaluation system 2004A; selecting chromatographic peaks existing in chromatograms of different batches of instant zizyphus jujube kernel xinning solid beverages as common peaks; generating a comparison fingerprint of the instant zizyphus jujube kernel xinning solid beverage by using an average value calculation method, and calculating the relative retention time and the relative peak area of each common peak; marking chemical components of peaks in the comparison fingerprint spectrum according to the retention time of the mixed reference solution chromatogram;

and 5, comparing the fingerprint spectrum of the instant solid beverage of zizyphus jujube renxinning obtained in the step 3 with the spectrum of the mixed standard substance, and identifying that the No. 8 peak in the instant solid beverage of zizyphus jujube renxinning is chlorogenic acid, the No. 9 peak is puerarin and the No. 26 peak is formononetin.

As a preferred scheme, the method for detecting the fingerprint of the instant zizyphus jujube renxinning solid beverage comprises the following steps of 1, the preparation method of the sample solution of the instant zizyphus jujube renxinning solid beverage comprises the following steps: taking 5g of 8 batches of instant zizyphus jujube kernel xinning solid beverage clear paste samples, placing the samples in a round bottom flask, adding 50ml of methanol, carrying out ultrasonic extraction for 30min, centrifuging the extract for 5min at 12000 rpm, and passing the supernatant through a 0.45-micrometer microporous filter membrane to obtain a test solution.

Preferably, the method for detecting the fingerprint of the instant zizyphus jujube kernel xinning solid beverage comprises the following steps of 2, preparing a mixed reference solution: precisely weighing chlorogenic acid, puerarin and formononetin as reference substances, placing in a volumetric flask, adding methanol to constant volume to scale, shaking, and making into mixed reference substance solution containing 0.1019mg/mL chlorogenic acid, 0.1008mg/mL puerarin and 0.1022mg/mL formononetin.

As a preferred scheme, in the above method for detecting the fingerprint of the instant zizyphus jujube kernel xinning solid beverage, in step 3, the liquid chromatography conditions are as follows: a chromatographic column: YMC-Pack ODS-A, mobile phase: acetonitrile and 0.1% phosphoric acid water, gradient elution, diode array detector, detection wavelength: 254nm, column temperature 30 ℃, flow rate 0.9mL/min, sample injection volume: 10 μ L, gradient elution procedure as follows:

preferably, the method for detecting the fingerprint of the instant zizyphus jujube kernel xinning solid beverage is characterized in that the fingerprint contains 26 peaks.

The method for detecting the fingerprint of the instant solid beverage of the zizyphus jujube kernel xinning drink comprises the following steps: 15-30 parts of spina date seed, 10-20 parts of ginseng, 12-24 parts of poria cocos, 7-14 parts of medlar, 5-10 parts of cinnamon, 7-14 parts of kudzu root, 5-10 parts of platycodon grandiflorum, 7-14 parts of Chinese date, 6-12 parts of lotus seed, 6-12 parts of lily, 5-10 parts of cassia seed, 5-10 parts of cape jasmine, 5-10 parts of liquorice and 5-10 parts of hawthorn.

As a preferred scheme, the method for detecting the fingerprint spectrum of the instant zizyphus jujube renxinning solid beverage comprises the following steps: 15 parts of spina date seed, 10 parts of ginseng, 12 parts of poria cocos, 7 parts of medlar, 5 parts of cinnamon, 7 parts of radix puerariae, 5 parts of platycodon grandiflorum, 7 parts of Chinese date, 6 parts of lotus seed, 6 parts of lily, 5 parts of cassia seed, 5 parts of gardenia, 5 parts of liquorice and 5 parts of hawthorn.

Optimizing fingerprint detection conditions:

1. in the aspect of preparation optimization of sample solution

According to the invention, through experimental comparison of different extraction methods (ultrasonic extraction, reflux extraction, percolation extraction and the like) and different extraction solvents (methanol, water, 50% ethanol water solution, 70% ethanol, 95% ethanol and absolute ethanol), the results show that the spectrogram difference component obtained by ultrasonic extraction is relatively comprehensive, the extraction efficiency is high, the separation degree is good, so that the ultrasonic extraction method is adopted; in the investigation of the extraction solvent, the chromatogram of the methanol extract is found to have the most information content and the highest component content, so that methanol is selected for extraction.

2. In the aspect of optimizing chromatographic conditions

According to the invention, a diode array detector is adopted to inspect the detection wavelength, chromatograms at 205nm, 225nm, 254nm and 280nm are extracted, and when the detection wavelength is 254nm, the information content contained in the chromatograms is most comprehensive and the base line is stable, so 254nm is selected as the detection wavelength;

the method screens the flow rates (1mL/min, 0.9mL/min, 0.8mL/min and 0.6mL/min), and because the components in the instant zizyphus jujube benoxinning drink have better peak shapes and better separation effects at the flow rate of 0.9mL/min, the gradient condition with the flow rate of 0.9mL/min is finally selected.

The invention compares the elution effects of 5 different elution systems of methanol-water, acetonitrile-0.1% formic acid, acetonitrile-0.1% phosphoric acid water and acetonitrile-0.2% phosphoric acid water under different gradients. As a result, it was found that when acetonitrile and 0.1% phosphoric acid water were used as mobile phases, the separation effect of each component in the instant zizyphus jujube benoxinning solid beverage was good, and therefore acetonitrile and 0.1% phosphoric acid water were finally selected as mobile phases.

After the optimal fluidity composition is determined, the optimal gradient elution program is screened through a large number of experiments, and experiments show that when acetonitrile with the volume of 5% is adopted for 0-5 min; 5-25 min acetonitrile volume 5% -15%; the volume of acetonitrile is 15-30% in 25-70 min; the volume of acetonitrile is 30-35% in 70-80 min; the volume of acetonitrile is 35-100% in 80-100 min; good separation degree of each spectrum peak in the fingerprint spectrum can be realized.

Has the advantages that:

1. according to the structural property characteristics of active ingredients contained in the instant zizyphus jujube kernel xinning solid beverage, the optimal mobile phase composition is screened out through a large number of experiments, and analysis conditions such as gradient elution procedures, flow rate, detection wavelength, chromatographic column, column temperature and the like are verified through a plurality of experiments.

2. The method for detecting the fingerprint spectrum of the instant solid beverage of the zizyphus jujube kernel xinning provided by the invention can comprehensively, objectively and accurately detect and evaluate the quality of the instant solid beverage of the zizyphus jujube kernel xinning, and has important significance for ensuring the curative effect of the instant solid beverage of the zizyphus jujube kernel xinning.

3. The fingerprint of the instant solid beverage of the wild jujube kernel xinning established by the method can effectively characterize the quality of the instant solid beverage of the wild jujube kernel xinning, objectively embody the front and back sequence and the mutual relation of each fingerprint characteristic peak, pay attention to the overall appearance characteristic, avoid the one-sidedness of the quality of the instant solid beverage of the wild jujube kernel xinning determined by measuring individual chemical components, and reduce the possibility of manual treatment for reaching the quality standard.

4. The method for detecting the fingerprint of the instant zizyphus jujube benoxinning solid beverage provided by the invention has the advantages of simple method, good stability, high precision, good reproducibility and the like.

Drawings

FIG. 1 is a chromatogram of a mixed control according to the present invention.

Fig. 2 is a comparative fingerprint of a sample of the instant zizyphus jujube renxinning solid beverage of the present invention.

Fig. 3 shows the fingerprint of 8 batches of the instant zizyphus jujube kernel xinning solid beverage sample.

Detailed Description

Embodiments of the present invention will be described in detail with reference to examples, in which specific conditions are not specified, according to conventional conditions or conditions recommended by manufacturers. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.

The following examples used the following instruments and reagents:

experimental equipment

1.1 instruments

A high-performance liquid chromatography system with full-wave-band scanning (200- & 800nm) of Shimadzu corporation in Japan comprises a full-automatic online degassing system, a full-automatic sample introduction system promience SIL-20A, a diode array detector SPD-M20A, an automatic temperature control column oven CTO-20A, a KQ3200DB type numerical control ultrasonic cleaner (ultrasonic instruments Co., Ltd., Kunshan city) and a BP121S electronic analysis balance (SARTORIUS).

1.2 drugs and reagents

The instant zizyphus jujube benxinning solid beverage sample comes from Jiangsu Haihong pharmaceutical Co Ltd; chlorogenic acid reference (batch No. 110753-201314) was purchased from China food and drug Biometrics institute; puerarin reference substance (batch No. 3681-99-0) is purchased from China food and drug institute, formononetin reference substance (batch No. 111703-.

Embodiment 1 a method for detecting a fingerprint of an instant zizyphus jujube kernel xinning solid beverage, comprising the following steps:

step 1, preparing an instant zizyphus jujube benxinning solid beverage test solution:

taking 20g of 8 batches of instant spina date seed, ginseng 2g, poria cocos 2.4g, medlar 1.4g, cinnamon 1g, kudzu vine root 1.4g, platycodon grandiflorum 1g, Chinese date 1.4g, lotus seed 1.2g, lily 1.2g, cassia seed 1g, gardenia 1g, liquorice 1g and hawthorn 1g, putting the sample in a 500mL round-bottom bottle, adding 250mL of methanol solution, carrying out ultrasonic extraction for 30min, centrifuging 12000 for 5min, taking supernatant, and filtering the supernatant through a 0.45 mu m microporous filter membrane to obtain a test solution;

step 2, preparation of mixed reference solution:

precisely weighing chlorogenic acid, puerarin and formononetin as reference substances, placing in a volumetric flask, adding methanol to constant volume to scale, shaking, and making into mixed reference substance solution containing 0.1019mg/mL chlorogenic acid, 0.1008mg/mL puerarin and 0.1022mg/mL formononetin.

Respectively and precisely sucking 8 batches of the instant zizyphus jujube renxinning solid beverage sample solution and the mixed reference substance solution, injecting the sample solution and the mixed reference substance solution into a high performance liquid chromatograph, and recording a chromatogram; the liquid chromatography conditions were: a chromatographic column: YMC-Pack ODS-A, mobile phase: acetonitrile and 0.1% phosphoric acid water, gradient elution, diode array detector, detection wavelength: 254nm, column temperature 30 ℃, flow rate 0.9mL/min, sample injection volume: 10 μ L, gradient elution procedure as follows:

Procedure time (min) Acetonitrile volume (%)
1 0 5
2 5 5
3 25 15
4 70 30
5 80 35
6 100 100

Step 4, exporting the fingerprints of the 8 batches of instant zizyphus jujube renxinning solid beverage test solution obtained in the step 3, and importing the fingerprints into a traditional Chinese medicine chromatography fingerprint similarity evaluation system 2012A; selecting chromatographic peaks existing in chromatograms of 8 batches of instant zizyphus jujube kernel xinning solid beverages as common peaks; generating a contrast fingerprint of 1 batch of instant zizyphus jujube benoxinning solid beverage by using an average value calculation method, and calculating the relative retention time and the relative peak area of each common peak; results 1 batch of the crude instant zizyphus jujube renxinning solid beverage had 27 common peaks, the reference fingerprint is shown in fig. 2, and the fingerprint of 8 batches of the test article is shown in fig. 3. The retention time of chlorogenic acid is 25.235min, puerarin is 28.92min, and formononetin is 87.547 min.

Step 5, comparing the fingerprint spectrum of the instant solid beverage of zizyphus jujube benoxinning drink obtained in the step 3 with the spectrum of the mixed standard substance (figure 1), identifying the main components, and comparing the number 8, 9 and 26 chromatographic peaks in the instant solid beverage of zizyphus jujube benxinning drink to be respectively as follows: chlorogenic acid (retention time 25.235min), puerarin (retention time 28.92min), and formononetin (retention time 87.547 min).

Meanwhile, the invention uses the automatically generated reference HPLC fingerprint spectrum R to generate a common chromatographic peak mode, and the common chromatographic peaks of 8 batches of instant solid beverage Chinese medicinal materials of the Zizyphus jujube Rexinning drink obtained by analysis and calculation have relatively good similarity, which shows that the fingerprint spectrum established by the instant solid beverage Chinese medicinal materials of Zizyphus jujube Rexinning drink established by the method can well detect the quality of multiple batches of instant solid beverage of Zizyphus jujube Rexinning drink in the Jiangsu Heishao pharmaceutical industry, and the results are shown in Table 1.

TABLE 1 similarity between batches of samples and consensus patterns

S1 S2 S3 S4 S5 S6 S7 S8 R
S1 1.000 0.958 0.991 1.000 0.995 0.991 0.987 0.958 0.994
S2 0.958 1.000 0.965 0.958 0.955 0.965 0.981 1.000 0.980
S3 0.991 0.965 1.000 0.991 0.991 1.000 0.987 0.965 0.995
S4 1.000 0.958 0.991 1.000 0.995 0.991 0.987 0.958 0.994
S5 0.995 0.955 0.991 0.995 1.000 0.991 0.983 0.955 0.993
S6 0.991 0.965 1.000 0.991 0.991 1.000 0.987 0.965 0.995
S7 0.987 0.981 0.987 0.987 0.983 0.987 1.000 0.981 0.996
S8 0.958 1.000 0.965 0.958 0.955 0.965 0.981 1.000 0.980
R 0.994 0.980 0.995 0.994 0.993 0.995 0.996 0.980 1.000

Example 2 methodological studies of fingerprint detection:

1. methodology investigation

1.1 precision investigation

Taking 20g of an instant zizyphus jujube benoxinning solid beverage sample (same as example 1), preparing a sample solution according to the sample preparation method of the example 1, carrying out continuous sample injection for 6 times, wherein the sample injection amount is 10 mu L each time, detecting according to the chromatographic conditions of the example 1, determining an HPLC chromatogram, and inspecting 27 common fingerprint peaks in the chromatogram, wherein the results show that the retention time RSD of the common fingerprint peaks is less than 1.5%, the common peak area RSD is less than 2.8%, and the precision of the instrument is better.

1.2 stability Studies

Taking 20g of an instant zizyphus jujube benoxinning solid beverage sample (same as example 1), preparing a test sample solution according to the test sample preparation method of the example 1, injecting samples for 0, 2, 4, 8, 12 and 24 hours according to the chromatographic conditions in the example 1, recording a chromatogram, and inspecting 27 common fingerprint peaks in the chromatogram, wherein the results show that the retention time RSD of the common fingerprint peaks is less than 1.0 percent, the common peak area RSD is less than 2.7 percent, and the test sample solution has better stability within 24 hours.

1.3 repeatability test

Taking 20g of 6 parts of instant zizyphus jujube kernel xinning solid beverage sample (same as example 1), preparing a sample solution according to the sample preparation method of the example 1, respectively measuring, recording a chromatogram, and inspecting 27 common fingerprint peaks in the chromatogram, wherein the results show that the retention time RSD of the common fingerprint peaks is less than 0.9 percent, and the area RSD of the common fingerprint peaks is less than 2.4 percent, which indicates that the method has good repeatability.

The experimental results show that the fingerprint spectrum detection method for the instant zizyphus jujube solid beverage for renxinning provided by the invention has the advantages of good stability, high precision and good repeatability, can comprehensively and objectively evaluate the quality of the instant zizyphus jujube solid beverage for renxinning, and has important significance for ensuring the clinical curative effect.

The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.

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