CN113960234A

CN113960234A - Quality control method for cynanchum glaucescens and cynanchum glaucescens formula granules

Info

Publication number: CN113960234A
Application number: CN202111101636.1A
Authority: CN
Inventors: 张志强; 沈建梅; 杜微波; 万莹莹; 付静
Original assignee: Beijing Tcmages Pharmaceutical Co Ltd
Current assignee: Beijing Tcmages Pharmaceutical Co Ltd
Priority date: 2021-09-18
Filing date: 2021-09-18
Publication date: 2022-01-21
Anticipated expiration: 2041-09-18
Also published as: CN113960234B

Abstract

The invention provides a quality control method of cynanchum glaucescens and cynanchum glaucescens formula granules, which comprises the steps of obtaining a test sample of cynanchum glaucescens and preparing a test sample solution, and obtaining a characteristic map of the test sample solution by adopting a high performance liquid chromatography, wherein the characteristic map at least comprises chromatographic peaks corresponding to uridine, adenosine and tryptophan; the characteristic map further comprises: when the characteristic peak of uridine is used as the reference peak S, the relative retention time is within. + -. 10% of the predetermined values of 1.4 and 1.9. The quality of the cynanchum glaucescens formula granules is judged more accurately and objectively by the invention, so that the quality control requirement of clinical medication is met, and the effectiveness of clinical medication is ensured.

Description

Quality control method for cynanchum glaucescens and cynanchum glaucescens formula granules

Technical Field

The invention relates to the field of quality control of traditional Chinese medicines, in particular to a quality control method of cynanchum glaucescens and cynanchum glaucescens formula granules.

Background

Dried rhizome and root of Cynanchum bungei Cynanchum Stauntonii (Decne.) Schltr. ex L é vi. or Cynanchum genkwa Cynanchum glaucescens (Decne.) hand-Mazz. of Michelia of China pharmacopoeia (2020 edition) mainly have the functions of lowering qi, eliminating phlegm and relieving cough. The chemical components of cynanchum glaucescens are complex and mainly contain chemical components such as steroidal saponins, alkaloids, volatility, flavonoids, amino acids and the like.

The steroid saponins are used as main characteristic and functional components of cynanchum glaucescens and have stronger antiviral, anti-infection and anti-tumor activities. The steroid saponin components are obtained by silica gel column chromatography, eluting and enriching with high concentration alcohol and mixed organic solvent, and the water extract has very low content. However, the clinical medication of cynanchum glaucescens mostly adopts the form of decoction, so that the basis of the curative effect of cynanchum glaucescens is mainly water-soluble components, and researches show that the cynanchum glaucescens aqueous extract has stronger physiological activities of eliminating phlegm, resisting inflammation, resisting thrombus, relaxing trachea and the like. Therefore, the quality control is carried out on the water-soluble components in cynanchum glaucescens, the requirements of clinical medication are met, and the safety and the effectiveness of the medication can be better ensured.

At present, no quality control research report for controlling the quality of water-soluble components before bleaching is found.

Disclosure of Invention

Accordingly, the present invention provides a method for overall quality control of water-soluble components of cynanchum glaucescens.

A quality control method for BAIQIAN and BAIQIAN formula granule comprises obtaining sample of BAIQIAN and preparing into sample solution, and performing high performance liquid chromatography to obtain characteristic spectrum of the sample solution, wherein the characteristic spectrum at least comprises chromatographic peaks corresponding to uridine, adenosine and tryptophan.

And calculating the relative retention time of each characteristic peak and the reference peak S by taking the characteristic peak of the uridine as the reference peak S, wherein the characteristic map further comprises the characteristic peaks with the relative retention time within a specified value of 1.4 +/-10%.

And calculating the relative retention time of each characteristic peak and the reference peak S by taking the characteristic peak of the uridine as the reference peak S, wherein the characteristic map further comprises the characteristic peaks with the relative retention time within a specified value of 1.9 +/-10%.

Wherein the tryptophan corresponds to a relative retention time within + -10% of a defined value of 3.7 and the adenosine corresponds to a relative retention time within + -10% of a defined value of 4.1.

The chromatographic conditions of the high performance liquid chromatography are as follows:

a chromatographic column: a chromatographic column using phenyl-hexyl silane bonded silica gel as a filler; detection wavelength: 205nm-280 nm; methanol is used as a mobile phase A, water is used as a mobile phase B, and elution is carried out according to the following gradient elution procedure:

the column temperature of the chromatographic column in the high performance liquid chromatography is 28-32 ℃, the flow rate is 0.8-1.2ml/min, and the number of theoretical plates is not less than 3000 calculated according to tryptophan.

The test sample for Cynanchum glaucescens is Cynanchum glaucescens medicinal material, decoction pieces of Cynanchum glaucescens, water extract of Cynanchum glaucescens or granule of Cynanchum glaucescens formula, wherein the water extract of Cynanchum glaucescens is water extractive solution of Cynanchum glaucescens, water extractive concentrated solution of Cynanchum glaucescens, and water extractive dry powder of Cynanchum glaucescens.

The preparation process of the test solution comprises the following steps: taking a test sample, adding a solvent, uniformly mixing, sealing, weighing, pretreating, cooling, weighing again, complementing the weight loss by the solvent, uniformly shaking, and filtering to obtain a filtrate, wherein the filtrate is a test sample solution;

when the sample is cynanchum glaucescens or cynanchum glaucescens decoction pieces, the pretreatment mode is heating reflux; when the test sample is a swallowwort extraction or a swallowwort formula particle, the pretreatment mode is ultrasonic treatment.

The solvent is methanol water solution with the mass concentration of 0-100% or ethanol water solution with the mass concentration of 0-100%. That is, the solvent may be pure water, methanol, ethanol, an aqueous methanol solution or an aqueous ethanol solution.

The power of the ultrasonic treatment is 250-300W, the frequency is 40kHz, and the time of the ultrasonic treatment is 15-45 min; heating and refluxing for 15-45 min; the preferred solvent is methanol at a mass concentration of 70%.

The invention also comprises quantitative control of the content of tryptophan in the swallowwort prescription granule, which comprises controlling the content of the tryptophan in the swallowwort prescription granule to be 0.12 mg/g-0.65 mg/g.

The content of the tryptophan is detected by adopting a high performance liquid chromatography, the detection wavelength of the high performance liquid chromatography is 218nm, and other conditions are the same as the characteristic spectrum.

The technical scheme of the invention has the following advantages:

1. the quality control method provided by the invention realizes the common control of the evaluation index components of uridine, tryptophan and adenosine simultaneously, achieves the aim of the overall quality control of the cynanchum glaucescens and cynanchum glaucescens formula granules, can judge the quality of the cynanchum glaucescens formula granules more accurately and objectively, meets the quality control requirement of clinical medication, and ensures the effectiveness of clinical medication.

2. The invention further optimizes the chromatographic conditions for obtaining the characteristic spectrum, including the optimization of the mobile phase and the optimization of the gradient elution program, can effectively improve the peak shape and the chromatographic peak separation degree, and can achieve the effects of high efficiency, sensitivity and accuracy in detection.

3. The invention also carries out quantitative control aiming at the content of the tryptophan, namely, the content of the tryptophan in the swallowwort prescription granule is controlled to be 0.12mg/g to 0.65 mg/g; in addition, the method can also effectively realize the quality control of the substance transfer process, and specifically comprises the following steps: the quality control of intermediate products (extracting solution, concentrated solution and dry powder) in the preparation process of the prescription granule can be effectively realized, and the components of the finally prepared cynanchum glaucescens prescription granule can be basically consistent with that of the standard decoction freeze-dried powder.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.

FIG. 1 is a characteristic map of a swallowwort formulation granule in example 1 of the present invention.

FIG. 2 is a characteristic diagram of a reference solution and a test solution in example 1 of the present invention.

FIG. 3 is a characteristic diagram of swallowwort decoction pieces and swallowwort prescription granules in example 1 of the present invention.

FIG. 4 is a fingerprint obtained upon repetitive detection in example 2 of the present invention.

FIG. 5 shows a fingerprint obtained in the detection of the specificity in embodiment 4 of the present invention.

FIG. 6 shows a fingerprint obtained in example 5 of the present invention.

FIG. 7 shows a fingerprint obtained in example 6 of the present invention.

FIG. 8 is a fingerprint spectrum of 280nm wavelength obtained in example 7 of the present invention.

FIG. 9 shows a fingerprint spectrum of 205nm wavelength obtained in example 6 of the present invention.

FIG. 10 is a fingerprint obtained in comparative example 1 of the present invention.

Detailed Description

The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.

The instrument comprises the following steps: shimadzu 2010AHT hplc; a UV ultraviolet detector; shimadzu 20AT high performance liquid chromatograph; a PDA ultraviolet detector; ME104E electronic balance (Mettler tolador), JY20002 electronic balance (Mettler tolador), KQ-300DB ultrasonic cleaner (Kunshan ultrasonic instruments Co., Ltd.); an electronic constant temperature water bath DZKW-4 (Beijing Zhongxing Weiwei instruments Co., Ltd.).

Reagent testing: uridine control (batch No. 110887-,

tryptophan control (batch No.: 140686-,

adenosine control (batch No. 110879) 201703, China institute for testing food and drug),

cynanchum glaucescens reference drug (willow leaf Cynanchum glaucescens) (batch No. 121442-201002, China institute for biological drug products),

baiqiang formula granule: the Baiqian formula particles are prepared by the Baiqian decoction pieces with the batch numbers of 200327-.

Reagent: methanol (SUPELCO) is used as chromatographic pure, methanol (national drug group chemical reagent Co., Ltd.) is used as analytical pure, and water is Drech purified water.

Example 1

A quality control method for BAIQIAN and BAIQIAN formula granule comprises obtaining sample of BAIQIAN and preparing into sample solution, and performing high performance liquid chromatography to obtain characteristic spectrum of the sample solution, wherein the characteristic spectrum at least comprises chromatographic peaks corresponding to uridine, adenosine and tryptophan. In particular, the method comprises the following steps of,

the chromatographic conditions of the high performance liquid chromatography in this example were: phenyl-hexylsilane bonded silica gel is used as a filler (the column length is 250mm, the column inner diameter is 4.6mm, and the particle size is 5 μm); methanol is taken as a mobile phase A, water is taken as a mobile phase B, and elution is carried out according to the specification in the following table 1; the flow rate was 1.0ml per minute; the column temperature is 30 ℃; the detection wavelength was 265 nm. The number of theoretical plates should not be less than 3000 calculated as tryptophan.

TABLE 1

The preparation process of the reference solution of the reference medicinal materials in the invention comprises the following steps: taking 2.0g of cynanchum glaucescens reference medicinal material, placing the cynanchum glaucescens reference medicinal material in an erlenmeyer flask, precisely adding 25ml of 70% methanol, sealing, weighing, ultrasonically treating (power 300W and frequency 40kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking up, filtering, and taking the subsequent filtrate as the reference solution of the reference medicinal material. Taking appropriate amount of uridine, tryptophan and adenosine reference substances, precisely weighing, adding methanol to obtain solutions containing 10 μ g of each 1ml, and shaking to obtain reference substance solutions.

When the test sample is a swallowwort dispensing granule, the preparation process of the test sample solution is as follows: taking a proper amount of a test sample, grinding, taking about 0.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 70% methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 300W, frequency 40kHz) for 30 minutes, taking out, cooling, weighing again, complementing the lost weight with 70% methanol, shaking up, filtering, and taking a subsequent filtrate as a test sample solution.

In this embodiment, 15 batches of cynanchum glaucescens decoction pieces are used to prepare cynanchum glaucescens formula granules for determination as a test sample, a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012.1 version) is used according to a liquid chromatogram of the obtained cynanchum glaucescens formula granules, an S1 liquid chromatogram in the 15 batches of liquid chromatograms is used as a reference chromatogram, a reference chromatogram is obtained by calculating a median, identification of common peaks is performed, and 5 common peaks are identified in total, as shown in fig. 1; and obtaining the retention time of each characteristic peak in the liquid phase map corresponding to each sample, and calculating the relative retention time of each characteristic peak at the same time, as shown in table 2.

TABLE 2

As can be seen from table 2: the relative retention time difference of each characteristic peak is small and is within the range of +/-10 percent, thereby meeting the quality control requirement.

And, one batch of the test solution and the reference solution of the reference substance are used for detection, the detection result is shown in figure 2, and by comparing the characteristic peaks in the uridine, tryptophan and adenosine reference solution and the test solution in figure 2, the peak 1 is uridine, the peak 4 is tryptophan and the peak 5 is adenosine. The preparation process of the reference substance solution of the reference substance comprises the following steps: respectively taking appropriate amount of uridine control, adenosine control and tryptophan control, precisely weighing, and adding methanol to obtain solutions containing 10 μ g of each 1ml of uridine control, adenosine control and tryptophan control, as control reference solutions.

Meanwhile, the cynanchum glaucescens formula granules prepared from one batch of cynanchum glaucescens decoction pieces and the batch of cynanchum glaucescens decoction pieces are detected, and the characteristic spectrum obtained by detection is shown in fig. 3. The process for preparing the test solution from cynanchum glaucescens decoction pieces comprises the following steps: precisely weighing about 1.0g of cynanchum glaucescens decoction pieces, placing in a conical flask with a plug, precisely adding 25ml of 70% methanol, sealing the plug, weighing, heating and refluxing for 15 min, taking out, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking, filtering, and collecting the subsequent filtrate as the sample solution.

Therefore, the quality control is carried out by determining the peak 1, the peak 4 and the peak 5 according to the peak correspondence of the characteristic peaks in the characteristic spectrum, so that the quality of cynanchum glaucescens can be effectively evaluated, and the reasonability of the evaluation method is ensured. Furthermore, a cynanchum glaucescens reference medicinal material is selected as a follow-up reference, the relative retention time is calculated by taking the No. 1 peak (uridine) as an S peak through the

characteristic peaks

2 and 3, and the quality control is performed by combining the relative retention time of the

characteristic peaks

2 and 3, so that the quality of the cynanchum glaucescens and the cynanchum glaucescens formula granules can be controlled integrally.

Example 2

In this example, the repeatability, the intermediate precision and the stability of the characteristic spectrum are verified as follows:

1. repeatability of

Taking 6 parts of the swallowwort formulation granules of the same batch, preparing a test solution according to the method in the example 1, and measuring to obtain a characteristic map shown as a figure 4, wherein the peak 1, the peak 4 and the peak 5 are considered to correspond to the chromatographic peak of a corresponding reference solution, the peak 2 and the peak 3 take the peak 1 as a reference peak, the relative retention time is calculated, and the RSD is calculated, and the results are shown as the following table 3:

TABLE 3

And (3) knotting: according to the repeatability investigation result, the

peaks

1, 4 and 5 have good correspondence with the corresponding reference substances, and the relative retention time RSD of the

characteristic peaks

2 and 3 is in the range of 0.0-0.1%, which indicates that the repeatability of the characteristic spectrum is good.

2. Intermediate precision

Using shimadzu 2010AHT and a UV ultraviolet detector, taking cynanchum glaucescens formula particles, preparing a sample solution according to the method in example 1, performing 6 times of measurement to obtain a characteristic map, calculating relative retention time by taking peak 1 as a reference peak, and calculating RSD, the results are shown in table 4 below.

TABLE 4 characteristic spectra intermediate precision survey retention time, relative retention time

And (3) knotting: in the characteristic maps obtained by adopting the Shimadzu 2010AHT and the UV ultraviolet detector, the

peaks

1, 4 and 5 have good correspondence with corresponding reference substances, and the relative retention time RSD of the

characteristic peaks

2 and 3 is within the range of 0.1%. The relative retention time RSD range of the

peaks

2 and 3 between different instruments is 0.0-0.9%, and the result shows that the characteristic spectrum result meets the analysis requirement between different instruments.

3. Stability of

Taking the swallowwort formulation granules, preparing a test solution according to the method in the example 1, respectively measuring at 0 hour, 2 hours, 4 hours, 8 hours, 12 hours and 24 hours according to a text method, obtaining a characteristic spectrum, respectively taking the peak 1 as a reference peak, calculating the relative retention time, and calculating the RSD, wherein the results are shown in the following table 5.

TABLE 5 feature Profile stability Retention time, relative Retention time

And (3) knotting: from the results of the stability experiment, the relative retention time RSD of each characteristic peak was in the range of 0.5%, indicating that the test article solution was stable within 24 hours.

Example 3

The method for controlling the quality of swallowwort rhizome formulation granules provided in this example comprises, in addition to the quality control of the characteristic map described in example 1, quantitative control of the quality evaluation index component in the swallowwort rhizome formulation granules, and comprises controlling the content of tryptophan in the swallowwort rhizome formulation granules to be 0.12mg/g to 0.65 mg/g.

The chromatographic conditions used in this example were substantially the same as those in example 1, except that the detection was carried out after the detection wavelength was adjusted to 218 nm.

Using the chromatographic conditions of this example, a tryptophan standard curve was first plotted to obtain a regression equation for tryptophan of y 26757x-678.37, R1.0000, and a linear range of 1.02-51.23 μ g/ml.

Then, the detection method of this example was used to detect 15 batches of cynanchum glaucescens decoction pieces, standard decoction, and 3 batches of formula granules, and the percentage content of tryptophan was calculated by substituting the detection results into the regression equation of tryptophan, with the calculation results shown in table 6.

TABLE 6

As can be seen from table 6 above: the content of tryptophan in the cynanchum glaucescens decoction pieces is 0.04 mg/g-0.15 mg/g, and the average value is 0.10 mg/g; the content of tryptophan in the standard decoction of cynanchum glaucescens is 0.23 mg/g-0.65 mg/g, and the average value is 0.44 mg/g; the tryptophan content in the three batches of granules is 0.14-0.16 mg/g, the average value is 0.15mg/g, according to the conditions of auxiliary material addition in the production process and the like, and considering the difference condition of raw materials, 80% of the average value is determined to be used as the lower limit of the content, 80% of the average value is selected as the lower limit of the content limit of the formula granules, and the upper limit is not changed (same as the upper limit of standard decoction), so that the content of the swallowwort formula granules is determined to be 0.12-0.65 mg/g.

Example 4

The embodiment provides a process for verifying the accuracy, repeatability, intermediate precision and specificity of the tryptophan content detection method, which comprises the following steps:

1 accuracy

Taking a proper amount of tryptophan reference substances, precisely weighing, and adding 70% methanol solution to prepare solution containing 12.715 μ g of tryptophan per 1 ml. 9 parts of formula particles, each of which is about 0.25g, are precisely weighed, 5ml, 10ml and 15ml of tryptophan reference substance solution are precisely and sequentially added into each of the three parts, 20ml, 15ml and 10ml of 70% methanol are respectively added into the three parts, the 70% methanol addition amount is 25ml, the rest operation is the same as the operation method of the example 3, the recovery rate is calculated according to the following formula, and the result is shown in the table 7.

TABLE 7 Tryptophan recovery test results Table

And (3) knotting: the recovery rate range of the tryptophan measured by a recovery rate test is 90.60-99.30%, the average recovery rate is 94.9%, the RSD value is 3.8%, and the recovery rate requirement is verified by a methodology, which shows that the result measured by the method is accurate.

2. Repeatability of

A test solution was prepared and measured by the method of example 3 using 6 parts of swallowwort dispensing granule, and the results of the measurements are shown in Table 8.

TABLE 8 Tryptophan content determination repeatability test

And (3) knotting: the average content of tryptophan measured by a repeatability test is 0.57mg/g, the RSD is 0.9 percent, and the requirement of methodology for verifying the repeatability is met.

3. Intermediate precision

Different analysts detect the same cynanchum glaucescens formula particles by different instruments at different times, and the instruments adopt an Shimadzu 2010AHT liquid chromatograph (UV ultraviolet detector) to perform intermediate precision tests. The following text shows the results of measurement of 6 parts of the formulation granules shown in Table 9.

TABLE 9 measurement of Tryptophan content intermediate precision test

And (3) knotting: the average content of tryptophan measured by the intermediate precision test is 0.56mg/g, the RSD value is 0.8 percent, and the RSD value of the detection result of the repeatability test is 0.7 percent, thereby meeting the requirement of methodology verification precision.

4. Specificity

The chromatogram of the test solution, the tryptophan control solution, and the negative control solution (70% methanol solution) was obtained as in example 3, and as shown in FIG. 5, it can be seen from FIG. 5 that the method was highly specific and the negative control was not interfered.

5. Stability of

The test solution was prepared from swallowwort dispensing granules according to the method of example 3, and the measurement was carried out for 0, 2, 4, 8, 12, and 24 hours, and the change of the tryptophan peak area was recorded, and the measurement results are shown in table 10.

Watch 10

From the above data, the peak area RSD of tryptophan within 24 hours was 2.7%, which was in accordance with the analytical requirements.

Example 5

In this example, standard spectra obtained at different column temperatures were examined, the other conditions were exactly the same as in example 3, specifically, the measurement was performed at column temperatures of 28 ℃, 30 ℃ and 32 ℃, the fingerprint obtained in this example is shown in fig. 6, and the content of tryptophan obtained by the detection is shown in table 11.

TABLE 11

The RSD value of the tryptophan content measured at different column temperatures is 2.6 percent, and the system applicability requirement is met. The method is shown to have better durability to different column temperatures.

Example 6

In this example, standard spectra obtained at different flow rates were examined, the other conditions were exactly the same as in example 3, specifically, the measurement was performed at flow rates of 0.8ml/min, 1.0ml/min, and 1.2ml/min, the fingerprint obtained in this example is shown in fig. 7, and the content of tryptophan obtained by detection is shown in table 12.

TABLE 12

The RSD value of the tryptophan content measured at different flow rates is 1.8 percent, and the system applicability requirement is met. Indicating that the method is more robust to different flow rates.

Example 7

In this example, standard spectra obtained under different wavelengths were examined, the other conditions were exactly the same as in example 3, specifically, the measurement was performed at wavelengths of 205nm and 280nm, and the fingerprints obtained in this example are shown in fig. 8 and 9, in which fig. 8 is a fingerprint at a wavelength of 280nm, and fig. 9 is a fingerprint at a wavelength of 205 nm.

Comparative example 1

This example provides another method for quality control under chromatographic conditions, which specifically comprises the following steps:

when the same test sample as in example 1 was used for quality control, the chromatographic conditions of this comparative example were: phenyl-hexyl silane bonded silica gel is used as a filling agent; acetonitrile-water (4:96) is used as a mobile phase; the flow rate was 0.8ml per minute; the column temperature is 30 ℃; the detection wavelength is 224nm, and the number of theoretical plates is not less than 3000 calculated according to tryptophan.

The results of the detection under the chromatographic conditions are shown in FIG. 10, and it can be seen from FIG. 10 that: the obtained sample has uneven base line of chromatogram, and bad peak shape of tryptophan, adenosine, and uridine chromatogram, which is not good for quality control of rhizoma Cynanchi Stauntonii granule.

It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims

1. A quality control method for rhizoma Cynanchi Stauntonii and rhizoma Cynanchi Stauntonii formula granules is characterized by comprising the steps of obtaining a test sample of the rhizoma Cynanchi Stauntonii and preparing the test sample solution, and obtaining a characteristic map of the test sample solution by adopting a high performance liquid chromatography, wherein the characteristic map at least comprises chromatographic peaks corresponding to uridine, adenosine and tryptophan.

2. The method for controlling the quality of Bai Qian and Bai Qian formula granules according to claim 1, wherein the characteristic peak of uridine is used as the reference peak S, the relative retention time of each characteristic peak and the reference peak S is calculated, and the characteristic map further comprises the characteristic peak with the relative retention time within the specified value of 1.4 ± 10%.

3. A method for controlling the quality of Bai Qian and Bai Qian formula granules according to claim 1 or 2, wherein the characteristic peak of uridine is used as the reference peak S, the relative retention time of each characteristic peak and the reference peak S is calculated, and the characteristic map further comprises the characteristic peaks with the relative retention time within the specified value of 1.9 ± 10%.

4. A method for quality control of swallowwort and swallowwort formulation granules according to any one of claims 1 to 3, wherein the chromatographic conditions of the high performance liquid chromatography are:

a chromatographic column: a chromatographic column using phenyl-hexyl silane bonded silica gel as a filler; detection wavelength: 205nm-280 m; methanol is used as a mobile phase A, water is used as a mobile phase B, and elution is carried out according to the following gradient elution procedure:

5. the method for controlling the quality of cynanchum glaucescens and cynanchum glaucescens formula granules according to claim 4, wherein the column temperature of a chromatographic column in the high performance liquid chromatography is 28-32 ℃, the flow rate is 0.8-1.2ml/min, and the number of theoretical plates is not less than 3000 calculated according to tryptophan.

6. The method for controlling the quality of BAIJIAO and BAIJIAO granule as claimed in any one of claims 1-5, wherein the sample for BAIJIAO is BAIJIAO crude drug, BAIJIAO decoction pieces, BAIJIAO water extract or BAIJIAO granule, wherein the BAIJIAO water extract is BAIJIAO water extractive solution, BAIJIAO water extractive concentrated solution, BAIJIAO water extractive dried powder.

7. The quality control method of cynanchum glaucescens and cynanchum glaucescens formula granules as claimed in claim 6, wherein the preparation process of the test solution is as follows: taking a test sample, adding a solvent, uniformly mixing, sealing, weighing, pretreating, cooling, weighing again, complementing the weight loss by the solvent, uniformly shaking, and filtering to obtain a filtrate, wherein the filtrate is a test sample solution;

when the sample is cynanchum glaucescens or cynanchum glaucescens decoction pieces, the pretreatment mode is heating reflux; when the test sample is a swallowwort extraction or a swallowwort formula particle, the pretreatment mode is ultrasonic treatment;

the solvent is methanol water solution with the mass concentration of 0-100% or ethanol water solution with the mass concentration of 0-100%.

8. The method as claimed in claim 7, wherein the power of the ultrasonic treatment is 250-300W, the frequency is 40kHz, and the time of the ultrasonic treatment is 15-45 min; the heating reflux time is 15-45 min.

9. The quality control method of rhizoma Cynanchi Stauntonii and rhizoma Cynanchi Stauntonii formulation granule according to any one of claims 1 to 8, further comprising quantitative control of tryptophan content in the rhizoma Cynanchi Stauntonii formulation granule, including controlling tryptophan content in the rhizoma Cynanchi Stauntonii formulation granule to be 0.12 mg/g-0.65 mg/g.

10. The method for quality control of rhizoma Cynanchi Stauntonii and rhizoma Cynanchi Stauntonii granule according to claim 9, wherein the content of tryptophan is detected by high performance liquid chromatography with the same characteristic spectrum.