CN113884591A - Method for controlling material quality and quantity of bitter orange - Google Patents
Method for controlling material quality and quantity of bitter orange Download PDFInfo
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Abstract
The invention belongs to the technical field of quality control of traditional Chinese medicines, and particularly relates to a method for comprehensively controlling the quality of medicinal materials by taking a fructus aurantii reference medicinal material as a reference substance and establishing a method independent of a reference substance. Determining the truth, namely the quality, of the fructus aurantii medicinal material by using the similarity of characteristic peaks of the fructus aurantii reference medicinal material and the fructus aurantii medicinal material to be detected; the internal standard components in the medicinal materials are accurately quantified, and the relative content of the characteristic peak of the bitter orange medicinal material is calculated by the internal standard components, so that the quality of the bitter orange medicinal material, namely the quantity, is determined. The method has good stability and precision, can make up for the deficiency of quality control of the traditional fructus Aurantii medicinal material, is beneficial to the problem that index components in the quality control of the fructus Aurantii medicinal material can not scientifically reflect the authenticity of the medicinal material, and can provide a new idea for improving the quality of the fructus Aurantii medicinal material.
Description
Technical Field
The invention belongs to the technical field of quality control of traditional Chinese medicines, and particularly relates to a method for comprehensively controlling the quality of medicinal materials by taking a fructus aurantii reference medicinal material as a reference substance, which is independent of a reference substance.
Background
The fructus Aurantii is Citrus aurantium of RutaceaeCitrus aurantium L. and its cultivars dried immature fruits mainly produced in Sichuan, Jiangxi and Zhejiang, and also distributed in Hubei, Hunan and Chongqing provinces. The original plants of the bitter orange have historically changed and are complex, and the clinical reasonable use of the traditional Chinese medicine bitter orange is influenced by the use of counterfeit products of green tangerine peel, trifoliate orange and the like as the bitter orange as a medicine.
With the progress of modern traditional Chinese medicine analysis means, the quality control method of the bitter orange mainly comprises a single-index content measurement method, a multi-index content measurement method and a fingerprint and content measurement combined method, the methods have the advantages of high sensitivity and good repeatability, and can provide quantitative data for controlling the bitter orange medicinal material, but the defects that the single index cannot reflect the integral characteristics of the medicinal material, the multi-index content measurement depends on various reference substances, certain index components cannot reflect the drug effect, and the fingerprint can only fuzzily evaluate the similarity of the medicinal material and cannot clearly judge the authenticity and quality of a test sample exist.
Disclosure of Invention
Aiming at the problems, the invention provides a method for controlling the quality-quantity dual-standard of a bitter orange medicament. The method is characterized in that the bitter orange reference medicinal material is used as a qualitative and quantitative reference substance, and a high performance liquid chromatography and Q-TOF-MS technology are combined to establish a set of method which does not depend on a reference substance and can comprehensively and scientifically control the quality of the medicinal material.
In order to achieve the above object, the present invention provides the following technical solutions.
The invention provides a method for controlling the material quality-quantity dual-standard of a bitter orange medicine, which is characterized by comprising the following steps of:
step 1, establishing a characteristic spectrum of the bitter orange medicinal material;
and 3, establishing the relative content of the characteristic peak of the bitter orange medicinal material.
Further, the specific steps of step 1 include:
(1) preparation of reference solutions: taking a fructus aurantii reference medicinal material, precisely weighing, placing into a conical flask with a plug, precisely adding 50 times of 50% methanol, weighing, heating and refluxing for 1h, cooling, complementing weight loss, shaking up, and filtering; volatilizing the filtrate, diluting with 50% methanol to desired volume, shaking, and filtering with 0.22 μm filter membrane to obtain the final product;
(2) preparation of a test solution: precisely weighing the powder of the test medicinal material passing through a No. 4 sieve, placing the powder in a conical flask with a plug, precisely adding 50 times of 50% methanol, weighing, heating and refluxing for 1h, cooling, weighing again, complementing the weight loss with 50% methanol, shaking up, and filtering; volatilizing the filtrate, diluting with 50% methanol to desired volume, shaking, and filtering with 0.22 μm filter membrane to obtain the final product;
(3) chromatographic conditions and system applicability test: agilent EC-C adopting octadecylsilane chemically bonded silica as filler18A chromatographic column with the specification of 3.0 multiplied by 100mm and 2.7-Micron; gradient elution is carried out by taking 0.1% formic acid water as a mobile phase A and acetonitrile as a mobile phase B; the flow rate is 1.0 mL/min; the column temperature is 30 ℃; the DAD detector detects at a wavelength of 330 nm; the sample injection amount is 5 mu L;
(4) characteristic spectrum: taking reference solution and sample solution, detecting according to chromatographic condition, and recording 330nm chromatogram.
Further, the specific steps of step 2 include:
taking the atlas of the fructus aurantii reference medicinal material as a reference spectrogram, automatically matching by using a median, performing multi-point correction, determining 20 common chromatographic peaks, and establishing the reference spectrogram of the fructus aurantii medicinal material; taking the established reference map as a reference, the contrast medicinal material of the fructus aurantii and 10 batches of test medicinal materials have 20 characteristic peaks, and the similarity between the contrast medicinal material and the test medicinal material and the reference map is more than 0.900-1.000, so that the characteristic peaks of the fructus aurantii medicinal materials are determined.
Further, the specific steps of step 3 include:
(1) the Q-TOF-MS technology is adopted to identify that 11 chemical components in 20 characteristic peaks of the bitter orange reference medicinal material characteristic spectrum are respectively eriocitrin at the No. 3 peak, neoeriocitrin at the No. 4 peak, naringin at the No. 6 peak, naringin at the No. 7 peak, hesperidin at the No. 9 peak, neohesperidin at the No. 10 peak, hesperetin at the No. 11 peak, poncirin at the No. 14 peak, hesperidin at the No. 15 peak, nobiletin at the No. 19 peak and hesperetin at the No. 20 peak; wherein, the No. 7 peak has good separation effect, large peak area and stable and centered retention time, so the No. 7 peak is used as a reference peak;
(2) preparing an internal standard substance solution, precisely weighing a proper amount of naringin, and preparing a solution containing 300 micrograms of a reference substance per 1mL by using methanol;
(3) taking the internal standard substance solution, determining according to the chromatographic conditions in the step 1, and calculating the naringin content of the fructus aurantii in the control medicinal material of 92.8753 mg/g and the peak area of 2547.697; the method for calculating the relative content of the characteristic peaks of the other 19 bitter orange medicinal materials comprises the following steps: characteristic peak relative content = characteristic peak area x (reference medicinal material naringin content/reference medicinal material naringin peak area);
(4) according to the relative content of the characteristic peaks of the fructus aurantii reference medicinal material and the test medicinal material, taking the average value-standard deviation as the lower limit of the characteristic peaks relative to the content of the internal standard.
Furthermore, the characteristic peaks of the step 2 are all characteristic active chemical components of the fructus aurantii playing the efficacy and pharmacological action.
Furthermore, the method can definitely identify the authenticity of the medicinal material by taking a characteristic peak in the characteristic spectrum of the bitter orange medicinal material as a qualitative standard of the bitter orange medicinal material.
Further, the method can distinguish the advantages and disadvantages of the bitter orange through the established lower limit of the relative content of each characteristic peak determined by the calculation method of the relative content of the characteristic peaks.
Compared with the prior art, the invention has the beneficial effects.
(1) The invention discloses a method for controlling the quality of a bitter orange medicament for the first time, which can overcome the defects that the single index in the existing method for controlling the quality of the bitter orange medicament cannot reflect the integral characteristics of the medicament, the multi-index content measurement depends on various reference substances, certain index components cannot reflect the medicament effect, and the fingerprint can only fuzzily evaluate the similarity of the medicament and cannot clearly judge the authenticity and quality of a test product.
(2) The invention utilizes modern analysis and detection technology to indicate that the basic parent nucleus of the chemical component of the characteristic peak is 2-phenyl chromone. Wherein the narirutin has antioxidant and small intestine promoting effects; naringin has biological activity of resisting gastric ulcer; hesperidin can promote gastrointestinal motility; neohesperidin has gastrointestinal hormone regulating effect; poncirin can inhibit gastric cancer cell proliferation; nobiletin has pharmacological effects of resisting inflammation and regulating gastrointestinal motility; the hesperetin has a certain treatment effect on colon cancer. The chemical components are all fructus aurantii, and the fructus aurantii plays roles of regulating qi, relieving epigastric distention, activating stagnancy and relieving flatulence, and has anti-inflammation and antioxidation functions. The active chemical components with pharmacological action of resisting cancer can comprehensively and scientifically reflect the internal quality of the traditional Chinese medicine bitter orange.
Drawings
FIG. 1 is a characteristic spectrum of a control material and 10 batches of test materials of fructus Aurantii.
Fig. 2 is a common pattern of the characteristic map of bitter orange.
FIG. 3 shows the characteristic maps of pericarpium Citri Tangerinae and fructus Aurantii as reference materials.
Detailed Description
The following examples will help to understand the present invention, but they are only for illustrative purposes and the present invention is not limited to these contents.
Example 1
Fructus Aurantii control drug (batch No. 120981-201605, China institute for testing and testing food and drug). The test sample of fructus Aurantii (Jiangxi Yichun, Jiangxi Jian, Jiangxi camphor tree, Zhejiang Quzhou, Zhejiang Jinhua, Sichuan Bazhong, Hunan Yuan Jiang, Chongqing Dabieshan, Hubei Xiaogan, Hebei Baoding) was identified as Ruxiang plant sour orange by Schenliang professor in Liaoning traditional Chinese medicine universityCitrus aurantium L.And dried unripe fruits of cultivars thereof. According to the detection method under the item of ' content determination ' of fructus Aurantii in ' pharmacopoeia of the people's republic of China ' 2020 edition, in 10 batches of production area samples, except the sample from filial pies in Hubei, the other samples can accord with the pharmacopoeia regulations (naringin content is not less than 4.0%, and neohesperidin content is not less than 3.0%).
1. Preparation of reference solutions:
taking 0.5g of fructus aurantii as a reference medicinal material, precisely weighing, placing in a conical flask with a plug, precisely adding 25mL of 50% methanol, weighing, heating and refluxing for 1h, cooling, complementing weight loss, shaking uniformly, and filtering. And (4) continuously volatilizing the filtrate, diluting the solution to a constant volume of 5mL by 50% methanol, shaking the solution uniformly, and filtering the solution through a 0.22 mu m filter membrane to obtain the product.
2. Preparation of a test solution:
taking 1.0g of test drug powder (screened by a No. 4 sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of 50% methanol, weighing, heating and refluxing for 1h, cooling, weighing again, complementing weight loss with 50% methanol, shaking up, and filtering. And (4) continuously volatilizing the filtrate, diluting the solution to a constant volume of 10mL by 50% methanol, shaking the solution uniformly, and filtering the solution through a 0.22-micron filter membrane to obtain the product.
3. And establishing a characteristic map.
3.1 chromatographic conditions and System suitability test:
a chromatographic column: agilent EC-C18Chromatography columns (3.0X 100mm, 2.7-Micron); mobile phase: 0.1% formic acid (A) -acetonitrile (B) was subjected to gradient elution; gradient elution procedure: 0-10 min, 5% → 15% B; 10-15 min, 15% → 18% B; 10-25 min, 18% → 50% B; flow rate: 1.0 mL/min; column temperature: 30 ℃; DAD detector wavelength: 330 nm; sample introduction amount: 5 μ L.
The quality control method of the traditional Chinese medicine fructus aurantii comprises the steps of enabling each sample of a test solution to be parallel for 2 times, sequentially carrying out sample injection detection according to chromatographic conditions, and leading out spectrum data under the wavelength of 330nm from an analytical detection instrument to obtain an HPLC (high performance liquid chromatography) characteristic spectrum of the fructus aurantii medicinal material, wherein the chart is shown in figure 1. Taking the chromatogram of the fructus Aurantii reference medicinal material as a reference chromatogram, automatically matching by using a median, performing multi-point correction, determining 20 common chromatographic peaks, and establishing the reference chromatogram of the fructus Aurantii medicinal material, wherein the chromatogram is shown in FIG. 2.
The method for controlling the quality of the bitter orange medicinal material can be used for judging the authenticity of the bitter orange medicinal material by the obtained bitter orange medicinal material characteristic spectrum.
3.2 methodological investigation.
3.2.1 precision experiment:
precisely absorbing 5 mu L of the same sample solution, determining according to chromatographic conditions, continuously injecting samples for 6 times, determining relative retention time and relative peak area of each chromatographic peak, and calculating relative standard deviation. The relative retention time of each chromatographic peak and the relative peak area RSD value are less than 1.0 percent, which indicates that the precision of the instrument is good.
3.2.2 stability experiments:
precisely sucking 5 μ L of the same sample solution, injecting sample for 6 times at 0, 2, 4, 8, 12, and 24h according to chromatographic conditions, measuring relative retention time and relative peak area of each chromatographic peak, and calculating relative standard deviation. The relative retention time of each chromatographic peak and the relative peak area RSD value are both less than 2.4 percent, which indicates that the test solution is stable within 24 hours.
3.2.3 repeatability experiments:
preparing 6 parts of test sample according to the preparation method of the test sample solution, respectively injecting and detecting according to chromatographic conditions, measuring the relative retention time and the relative peak area of each chromatographic peak, and calculating the relative standard deviation. The relative retention time of each chromatographic peak and the RSD value of the relative peak area are both less than 1.9 percent, which indicates that the method has good repeatability.
4. And (4) measuring the content.
4.1 Linear relationship examination:
preparing 6 solutions with mass concentration of naringin, respectively carrying out sample injection detection according to chromatographic conditions, drawing a standard curve by taking the mass (X) as a horizontal ordinate and the peak area (Y) as a vertical coordinate, and carrying out linear regression to obtain a linear regression equation (Y =1327.2X + 87.58), a correlation coefficient (r = 0.990) and a linear range (0.6800-5.7800 mu g). The result shows that the sample amount range and the peak area have good linear relation.
4.2 precision experiment:
precisely absorbing 5 mu L of the same sample solution, determining according to chromatographic conditions, continuously injecting samples for 6 times, determining relative retention time and relative peak area of each chromatographic peak, and calculating relative standard deviation. The relative retention time of each chromatographic peak and the relative peak area RSD value are both less than 2.2 percent, which indicates that the precision of the instrument is good.
4.3 stability test:
precisely sucking 5 μ L of the same sample solution, injecting sample for 6 times at 0, 2, 4, 8, 12, and 24h according to chromatographic conditions, measuring relative retention time and relative peak area of each chromatographic peak, and calculating relative standard deviation. The relative retention time of each chromatographic peak and the relative peak area RSD value are both less than 2.7 percent, which indicates that the test solution is stable within 24 hours.
4.4 repeatability experiments
Preparing 6 parts of test sample according to the preparation method of the test sample solution, respectively injecting and detecting according to chromatographic conditions, measuring the relative retention time and the relative peak area of each chromatographic peak, and calculating the relative standard deviation. The relative retention time of each chromatographic peak and the RSD value of the relative peak area are both less than 1.5 percent, which indicates that the method has good repeatability.
Calculating the relative content of characteristic peaks of the fructus aurantii control medicinal material and the rest 9 batches of fructus aurantii test medicinal materials except the Hubei filial piety fructus aurantii, and taking the average value-standard deviation as the lower limit of the characteristic peaks relative to the content of the internal standard. The content of the No. 1 characteristic peak is not less than 1.3975 mg/g; the content of the No. 2 characteristic peak is not less than 2.6439 mg/g; the content of the No. 3 characteristic peak is not less than 8.4466 mg/g; the content of the No. 4 characteristic peak is not less than 2.6317 mg/g; the content of the No. 5 characteristic peak is not less than 7.2282 mg/g; the content of the No. 6 characteristic peak is not less than 8.2781 mg/g; the content of the No. 8 characteristic peak is not less than 8.0920 mg/g; the content of the No. 9 characteristic peak is not less than 6.2699 mg/g; the content of the No. 10 characteristic peak is not less than 77.5915 mg/g; the content of the No. 11 characteristic peak is not less than 2.8459 mg/g; the content of the No. 12 characteristic peak is not less than 2.1630 mg/g; the content of the No. 13 characteristic peak is not less than 1.4016 mg/g; the content of the No. 14 characteristic peak cannot be lower than 1.4143 mg/g; the content of the No. 15 characteristic peak is not less than 1.3831 mg/g; the content of the No. 16 characteristic peak is not less than 1.3217 mg/g; the content of the No. 17 characteristic peak is not less than 2.4227 mg/g; the content of the No. 18 characteristic peak is not less than 6.7383 mg/g; the content of the No. 19 characteristic peak is not less than 1.5885 mg/g; the content of the characteristic peak No. 20 is not less than 5.1964 mg/g.
Example 2 identification of a counterfeit bitter orange medicinal material.
(1) Taking 1.0g of dried orange peel medicinal material powder (screened by a No. 4 sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of 50% methanol, weighing, heating and refluxing for 1h, cooling, weighing again, complementing weight loss with 50% methanol, shaking up, and filtering. The filtrate is continuously volatilized, 50 percent methanol is added to a 10mL volumetric flask, the volumetric flask is shaken up and filtered through a 0.22 mu m filter membrane for standby.
(2) Precisely sucking 5 mu L of the solution in the step (1), and injecting the solution into a liquid chromatograph under the following chromatographic conditions:
agilent EC-C using octadecylsilane chemically bonded silica as filler18A chromatographic column with the specification of 3.0 multiplied by 100mm and 2.7-Micron; gradient elution is carried out by taking 0.1% formic acid water as a mobile phase A and acetonitrile as a mobile phase B; the flow rate is 1.0 mL/min; the column temperature is 30 ℃; the DAD detector detects at a wavelength of 330 nm.
The dried orange peel is derived from citrus reticulata blanco of Rutaceae, and is a relatively common mixed variety of bitter orange medicinal materials. Compared with the characteristic spectrum of the fructus aurantii control medicinal material, the pericarpium citri reticulatae medicinal material does not have No. 5, No. 10, No. 14, No. 15, No. 16 and No. 17 characteristic peaks. By taking the characteristic peaks in the characteristic map of the bitter orange medicinal material as the qualitative standard of the bitter orange medicinal material, counterfeit products can be distinguished, the established characteristic map can identify the authenticity of the bitter orange medicinal material, and the problem of clinical medication confusion caused by citrus counterfeit products due to multiple fundamentals and multiple production places of the bitter orange can be solved, as shown in fig. 3.
Example 3 identification of a test sample of Hubei filial piety bitter orange.
(1) Preparation of reference solutions:
taking 0.5g of fructus aurantii as a reference medicinal material, precisely weighing, placing in a conical flask with a plug, precisely adding 25mL of 50% methanol, weighing, heating and refluxing for 1h, cooling, complementing weight loss, shaking uniformly, and filtering. And (4) continuously volatilizing the filtrate, diluting the solution to a constant volume of 5mL by 50% methanol, shaking the solution uniformly, and filtering the solution through a 0.22 mu m filter membrane to obtain the product.
(2) Preparation of a test solution:
taking 1.0g of test drug powder (screened by a No. 4 sieve), precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of 50% methanol, weighing, heating and refluxing for 1h, cooling, weighing again, complementing weight loss with 50% methanol, shaking up, and filtering. And (4) continuously volatilizing the filtrate, diluting the solution to a constant volume of 10mL by 50% methanol, shaking the solution uniformly, and filtering the solution through a 0.22-micron filter membrane to obtain the product.
(3) Sampling the test solution, detecting according to chromatographic conditions, recording a 330nm chromatogram, and presenting 20 characteristic peaks consistent with the characteristic spectrum of the fructus Aurantii reference medicinal material.
(4) And calculating the relative content of each characteristic peak of the Hubei filial tract bitter orange sample, wherein the relative content of the chemical components of the characteristic peaks = the peak area x of the characteristic peaks (naringin content of the reference medicinal material/naringin peak area of the reference medicinal material), wherein the relative content of the characteristic peaks 2, 5, 8, 10, 11, 12 and 13 is 0.4488mg/g, 0.4812mg/g, 1.8363mg/g, 7.3723mg/g, 0.3882mg/g, 1.1415mg/g and 1.1743mg/g respectively, and is lower than the lower limit.
Because the relativity of plants used as medicine of Rutaceae is very similar, if the citrus pseudodrug is used as bitter orange for a long time, the phenomena of difficult identification and disordered clinical medication are easy to cause. By taking the characteristic peaks in the characteristic map of the bitter orange as the qualitative standard of the bitter orange, counterfeit products can be distinguished obviously, the established characteristic map can identify the authenticity of the bitter orange, and the problem of clinical medication confusion caused by citrus counterfeit products due to multiple sources and multiple production places of the bitter orange can be solved. Early-stage efficacy experiments show that the test sample of Hubei filial piety bitter orange has no obvious effect on promoting gastrointestinal motility. The established lower limit of the relative content of the characteristic peak can distinguish the quality of the bitter orange, and can solve the problem of poor clinical efficacy of the poor bitter orange. The invention can clearly judge the quality of the sample, make up the deficiency of the quality control of the current bitter orange medicinal material and achieve the aim of comprehensively controlling the bitter orange medicinal material.
Claims (7)
1. A method for controlling the quality-quantity of a bitter orange medicine is characterized by comprising the following steps:
step 1, establishing a characteristic spectrum of the bitter orange medicinal material;
step 2, determining a characteristic peak of the bitter orange medicinal material;
and 3, establishing the relative amount of the characteristic peak of the bitter orange medicinal material.
2. The method for controlling the quality-quantity of a bitter orange drug according to claim 1, wherein the step 1 comprises the following steps:
(1) preparation of reference solutions: taking a fructus aurantii reference medicinal material, precisely weighing, placing into a conical flask with a plug, precisely adding 50 times of 50% methanol, weighing, heating and refluxing for 1h, cooling, complementing weight loss, shaking up, and filtering; volatilizing the filtrate, diluting with 50% methanol to desired volume, shaking, and filtering with 0.22 μm filter membrane to obtain the final product;
(2) preparation of a test solution: precisely weighing the powder of the test medicinal material passing through a No. 4 sieve, placing the powder in a conical flask with a plug, precisely adding 50 times of 50% methanol, weighing, heating and refluxing for 1h, cooling, weighing again, complementing the weight loss with 50% methanol, shaking up, and filtering; volatilizing the filtrate, diluting with 50% methanol to desired volume, shaking, and filtering with 0.22 μm filter membrane to obtain the final product;
(3) chromatographic conditions and system applicability test: agilent EC-C adopting octadecylsilane chemically bonded silica as filler18A chromatographic column with the specification of 3.0 multiplied by 100mm and 2.7-Micron; gradient elution is carried out by taking 0.1% formic acid water as a mobile phase A and acetonitrile as a mobile phase B; the flow rate is 1.0 mL/min; the column temperature is 30 ℃; the DAD detector detects at a wavelength of 330 nm; the sample injection amount is 5 mu L;
(4) characteristic spectrum: taking reference solution and sample solution, detecting according to chromatographic condition, and recording 330nm chromatogram.
3. The method for controlling the quality-quantity of a bitter orange drug according to claim 1, wherein the step 2 comprises the following steps:
taking the atlas of the fructus aurantii reference medicinal material as a reference spectrogram, automatically matching by using a median, performing multi-point correction, determining 20 common chromatographic peaks, and establishing the reference spectrogram of the fructus aurantii medicinal material; taking the established reference map as a reference, the contrast medicinal material of the fructus aurantii and 10 batches of test medicinal materials have 20 characteristic peaks, and the similarity between the contrast medicinal material and the test medicinal material and the reference map is more than 0.900-1.000, so that the characteristic peaks of the fructus aurantii medicinal materials are determined.
4. The method for controlling the quality-quantity of a bitter orange drug according to claim 1, wherein the step 3 comprises the following steps:
(1) the Q-TOF-MS technology is adopted to identify that 11 chemical components in 20 characteristic peaks of the bitter orange reference medicinal material characteristic spectrum are respectively eriocitrin at the No. 3 peak, neoeriocitrin at the No. 4 peak, naringin at the No. 6 peak, naringin at the No. 7 peak, hesperidin at the No. 9 peak, neohesperidin at the No. 10 peak, hesperetin at the No. 11 peak, poncirin at the No. 14 peak, hesperidin at the No. 15 peak, nobiletin at the No. 19 peak and hesperetin at the No. 20 peak; wherein, the No. 7 peak has good separation effect, large peak area and stable and centered retention time, so the No. 7 peak is used as a reference peak;
(2) preparing an internal standard substance solution, precisely weighing a proper amount of naringin, and preparing a solution containing 300 micrograms of a reference substance per 1mL by using methanol;
(3) taking the internal standard substance solution, determining according to the chromatographic conditions in the step 1, and calculating the naringin content of the fructus aurantii in the control medicinal material of 92.8753 mg/g and the peak area of 2547.697; the method for calculating the relative content of the characteristic peaks of the other 19 bitter orange medicinal materials comprises the following steps: characteristic peak relative content = characteristic peak area x (reference medicinal material naringin content/reference medicinal material naringin peak area);
(4) according to the relative content of the characteristic peaks of the fructus aurantii reference medicinal material and the test medicinal material, taking the average value-standard deviation as the lower limit of the characteristic peaks relative to the content of the internal standard.
5. The method for controlling the material quality and quantity of the fructus aurantii medicine according to claim 1, wherein the characteristic peaks in the step 2 are all characteristic active chemical components of the fructus aurantii playing the effect and pharmacological action.
6. The method for controlling the quality of a bitter orange drug according to claim 1, wherein the method can definitely identify the authenticity of the bitter orange drug by using a characteristic peak in a characteristic spectrum of the bitter orange drug as a qualitative standard of the bitter orange drug.
7. The method of claim 1, wherein the method is capable of distinguishing the quality of fructus Aurantii by determining the lower limit of the relative content of each characteristic peak by the established calculation method of the relative content of the characteristic peaks.
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Cited By (2)
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| CN115480001A (en) * | 2022-07-29 | 2022-12-16 | 丹东药业集团有限公司 | Herba epimedii particle two-dimensional multi-information reference internal standard quality control method |
| CN116990420A (en) * | 2023-09-27 | 2023-11-03 | 江西中医药大学 | Feature-map-based honey bran fructus aurantii comprehensive quality evaluation method |
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