CN115267007B - Method for establishing fingerprint of syrup for treating common cold and fever in children and fingerprint thereof - Google Patents
Method for establishing fingerprint of syrup for treating common cold and fever in children and fingerprint thereof Download PDFInfo
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- CN115267007B CN115267007B CN202210961570.1A CN202210961570A CN115267007B CN 115267007 B CN115267007 B CN 115267007B CN 202210961570 A CN202210961570 A CN 202210961570A CN 115267007 B CN115267007 B CN 115267007B
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- 239000006188 syrup Substances 0.000 title claims abstract description 95
- 235000020357 syrup Nutrition 0.000 title claims abstract description 95
- 201000009240 nasopharyngitis Diseases 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 29
- 206010037660 Pyrexia Diseases 0.000 title claims abstract description 28
- 230000001754 anti-pyretic effect Effects 0.000 claims abstract description 35
- 239000002221 antipyretic Substances 0.000 claims abstract description 35
- 239000012488 sample solution Substances 0.000 claims abstract description 34
- 239000003814 drug Substances 0.000 claims abstract description 28
- 239000000523 sample Substances 0.000 claims abstract description 22
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 19
- 239000012088 reference solution Substances 0.000 claims abstract description 13
- 238000011156 evaluation Methods 0.000 claims abstract description 7
- 238000004458 analytical method Methods 0.000 claims abstract description 6
- 238000002347 injection Methods 0.000 claims abstract description 6
- 239000007924 injection Substances 0.000 claims abstract description 6
- 230000014759 maintenance of location Effects 0.000 claims description 93
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- KFFCKOBAHMGTMW-LGQRSHAYSA-N Forsythin Chemical compound C1=C(OC)C(OC)=CC=C1[C@H]1[C@@H](CO[C@@H]2C=3C=C(OC)C(O[C@H]4[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O)=CC=3)[C@@H]2CO1 KFFCKOBAHMGTMW-LGQRSHAYSA-N 0.000 claims description 19
- 239000013558 reference substance Substances 0.000 claims description 13
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 7
- 238000011835 investigation Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000010231 banlangen Substances 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 238000010276 construction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 abstract description 21
- 239000000126 substance Substances 0.000 abstract description 9
- CRDNMYFJWFXOCH-YPKPFQOOSA-N (3z)-3-(3-oxo-1h-indol-2-ylidene)-1h-indol-2-one Chemical compound N/1C2=CC=CC=C2C(=O)C\1=C1/C2=CC=CC=C2NC1=O CRDNMYFJWFXOCH-YPKPFQOOSA-N 0.000 description 8
- 241000334154 Isatis tinctoria Species 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 235000004347 Perilla Nutrition 0.000 description 6
- 241000229722 Perilla <angiosperm> Species 0.000 description 6
- 229940079593 drug Drugs 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 241000334160 Isatis Species 0.000 description 5
- 240000000249 Morus alba Species 0.000 description 5
- 235000008708 Morus alba Nutrition 0.000 description 5
- 241001180876 Saposhnikovia Species 0.000 description 5
- CRDNMYFJWFXOCH-BUHFOSPRSA-N Couroupitine B Natural products N\1C2=CC=CC=C2C(=O)C/1=C1/C2=CC=CC=C2NC1=O CRDNMYFJWFXOCH-BUHFOSPRSA-N 0.000 description 4
- 241000576429 Forsythia suspensa Species 0.000 description 4
- 241000951473 Schizonepeta Species 0.000 description 4
- CRDNMYFJWFXOCH-UHFFFAOYSA-N isoindigotin Natural products N1C2=CC=CC=C2C(=O)C1=C1C2=CC=CC=C2NC1=O CRDNMYFJWFXOCH-UHFFFAOYSA-N 0.000 description 4
- 238000003908 quality control method Methods 0.000 description 4
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- 208000006820 Arthralgia Diseases 0.000 description 1
- 241000721047 Danaus plexippus Species 0.000 description 1
- 206010018498 Goitre Diseases 0.000 description 1
- 206010068319 Oropharyngeal pain Diseases 0.000 description 1
- 201000007100 Pharyngitis Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001647 drug administration Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 201000003872 goiter Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 210000001364 upper extremity Anatomy 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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Abstract
The invention discloses a method for establishing a syrup fingerprint spectrum for treating common cold and fever in children and the fingerprint spectrum. The establishing method comprises the following steps: 1) Preparing a sample solution and a reference solution; 2) Carrying out sample injection analysis on the sample solution and the reference solution by adopting HPLC (high performance liquid chromatography) to obtain an HPLC fingerprint of the sample solution; 3) And introducing the HPLC fingerprint data of the sample solution into 2012 edition of a traditional Chinese medicine fingerprint similarity evaluation system, taking 1 fingerprint of the sample solution as a reference spectrum, and generating a pediatric cold antipyretic syrup fingerprint reference spectrum by an average method. By applying the technical scheme of the invention, the fingerprint characteristic spectrum of the syrup for treating the common cold of the children generates 18 common peaks, can provide rich identification information, and can more comprehensively reflect the types and the amounts of chemical components contained in the syrup for treating the common cold of the children, thereby integrally describing and evaluating the quality of the syrup.
Description
Technical Field
The invention relates to the technical field of medicine analysis, in particular to a method for establishing a syrup fingerprint spectrum for treating common cold and fever in children and the fingerprint spectrum thereof.
Background
The syrup for treating the common cold and abating fever of children is a medicament for treating the common cold and abating fever of children, adopts bitter and cold dyers woad leaf and weeping forsythiae capsule as monarch drugs, has the effects of pungent and cool, pathogenic factors clearing and heat clearing, and has the effects of aromatic and dirt-removing and detoxifying; radix Isatidis helps folium Isatidis to clear heat and toxic materials, cool blood and relieve sore throat; ramulus Mori, herba Schizonepetae, fructus forsythiae, helps to dispel wind-heat, while Sang Zhiyou is indicated for arthralgia due to wind-dampness-heat of the upper limbs. The three medicines are ministerial medicines, and the perilla leaf, the divaricate saposhnikovia root and the fur opening of the product with less adjuvant and light clearing are used as ministerial medicines, so that the effects of dispelling wind and relieving exterior syndrome and clearing heat and detoxicating are achieved. The active ingredients of the traditional Chinese medicine composition comprise 150g of radix isatidis, 150g of fructus forsythiae, 150g of dyers woad leaf, 150g of mulberry twig, 60g of herba schizonepetae, 60g of radix sileris and 30g of perilla leaf by weight. It is a medicine with high bioavailability, complete absorption and obvious therapeutic effect for curing children's cold and defervescing.
The quality of the traditional Chinese medicine is related to clinical curative effect and safety, and establishing a quality control method of the traditional Chinese medicine is one of the key problems of the development of the traditional Chinese medicine. The fingerprint spectrum of the traditional Chinese medicine is a comprehensive and quantifiable chromatographic identification means, which is established on the basis of the research of the chemical components of the traditional Chinese medicine and can identify the uniformity and the stability of the quality of the finished product. The traditional Chinese medicine preparation is a multi-component complex system, so that the quality of the traditional Chinese medicine preparation is evaluated by adopting a detection method which is suitable for the traditional Chinese medicine preparation and can provide rich identification information, and the establishment of the traditional Chinese medicine fingerprint can reflect the types and the amounts of chemical components contained in the traditional Chinese medicine and the preparation more comprehensively, so that the overall description and the evaluation of the quality of the medicine are performed.
The fingerprint of the syrup for treating the common cold and reducing fever of the children takes the integral chemical characteristics of the medicine as a theoretical basis, thereby realizing the application of the syrup in the aspect of quality control. The characteristic is that the standardized procedure is used to obtain the extract of the characteristic total components of the medicine, and the HPLC means is used to characterize the composition and structure.
The quality control of the syrup for treating the common cold of children is carried out by referring to the national drug Standard (WS-11441 (ZD-1441) -2002-2012Z-2020) issued by the national drug administration at present, and detection is carried out by respectively selecting forsythin and indirubin as reference substances for identification, wherein the forsythin is used as the reference substance for identifying the forsythin medicinal material and the forsythin in the medicinal material, and the indirubin is used as the reference substance for identifying the isatis root and the dyers woad leaf in the medicinal syrup for treating the common cold of children.
Disclosure of Invention
The invention aims to provide a method for establishing the fingerprint of the syrup for treating the common cold and the fever of the children and the fingerprint thereof, which have high stability, good accuracy and good repeatability, can be used for monitoring the production process of the syrup for treating the common cold and the fever of the children, provides a certain theoretical basis and support for the establishment of a whole process quality control system, and ensures the safety and the effectiveness of clinical medication.
In order to achieve the above object, according to one aspect of the present invention, a method for establishing a fingerprint of a syrup for treating common cold and fever in children is provided. The establishing method comprises the following steps: 1) Preparing a sample solution and a reference solution; 2) Sample injection analysis is respectively carried out on the sample solution and the reference solution by adopting HPLC, so as to obtain the HPLC fingerprint of the sample solution; 3) And (3) introducing the HPLC fingerprint data of the sample solution into 2012 edition of a traditional Chinese medicine fingerprint similarity evaluation system, taking 1 fingerprint of the sample solution as a reference spectrum, and generating a pediatric cold antipyretic syrup fingerprint reference spectrum by an average method.
Further, preparing a test solution includes: weighing 5mL of the antipyretic syrup for treating the common cold of the children, placing in a 50mL volumetric flask, adding methanol, performing ultrasonic treatment for 30min, standing to a 50mL scale after reaching room temperature, shaking uniformly, filtering with a 0.45 μm microporous filter membrane, and taking the subsequent filtrate.
Further, preparing a reference solution includes: placing the forsythin reference substance into a volumetric flask, adding methanol to obtain solution containing 0.1mg of forsythin per 1mL, filtering with 0.45 μm microporous membrane, and collecting the filtrate.
Further, step 2) specifically includes: taking the same batch of sample solution of the syrup for treating common cold and fever of children, continuously injecting the sample for 6 times, and recording a chromatogram; taking the same batch of sample solutions of the infant cold antipyretic syrup, respectively injecting at 0,2,4,8 and 16 hours, and recording a chromatogram; simultaneously preparing N parts of sample solutions of the syrup for treating the common cold and fever of children, respectively injecting samples, and recording chromatograms, wherein N is more than or equal to 6.
Further, HPLC was performed using a Agilent ZORBAX SB-C18 column with a specification of 250mm by 4.6mm, 5. Mu.m; acetonitrile is taken as a mobile phase A, 0.1% phosphoric acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specifications in the following table;
the detection wavelength is 277nm; the column temperature is 30 ℃; the flow rate is 1.0ml per minute, and the theoretical plate number is not less than 3000 calculated according to the forsythin peak.
Further, the main components of the syrup for treating the common cold and fever of the children comprise: radix Isatidis, fructus forsythiae, folium Isatidis, ramulus Mori, herba Schizonepetae, radix Saposhnikoviae, and folium Perillae; preferably, the fingerprint of the antipyretic syrup for children in step 2) has 18 common chromatographic peaks, wherein the 18 peaks are respectively a peak 1 with a relative retention time of 0.128, a peak 2 with a relative retention time of 0.166, a peak 3 with a relative retention time of 0.201, a peak 4 with a relative retention time of 0.219, a peak 5 with a relative retention time of 0.230, a peak 6 with a relative retention time of 0.250, a peak 7 with a relative retention time of 0.290, a peak 8 with a relative retention time of 0.382, a peak 9 with a relative retention time of 0.508, a peak 10 with a relative retention time of 0.609, a peak 11 with a relative retention time of 0.634, a peak 12 with a relative retention time of 0.667, a peak 13 with a relative retention time of 0.717, a peak 14 with a relative retention time of 0.761, a peak 15 with a relative retention time of 0.916, a peak 16 with a relative retention time of 0.984, a peak with a relative retention time of 0.100, and a peak 18 with a relative retention time of 1.100.
According to another aspect of the invention, a child cold antipyretic syrup fingerprint obtained by the construction method of the child cold antipyretic syrup fingerprint is provided.
Further, it includes a peak No. 1 with a relative retention time of 0.128, a peak No. 2 with a relative retention time of 0.166, a peak No. 3 with a relative retention time of 0.201, a peak No. 4 with a relative retention time of 0.219, a peak No. 5 with a relative retention time of 0.230, a peak No. 6 with a relative retention time of 0.250, a peak No. 7 with a relative retention time of 0.290, a peak No. 8 with a relative retention time of 0.382, a peak No. 9 with a relative retention time of 0.508, a peak No. 10 with a relative retention time of 0.609, a peak No. 11 with a relative retention time of 0.634, a peak No. 12 with a relative retention time of 0.667, a peak No. 13 with a relative retention time of 0.717, a peak No. 14 with a relative retention time of 0.761, a peak No. 15 with a relative retention time of 0.916, a peak No. 16 with a relative retention time of 0.984, a peak No. 17 with a relative retention time of 0.100, and a peak No. 18 with a relative retention time of 1.376.
According to still another aspect of the invention, the application of the fingerprint spectrum of the syrup for treating the common cold of the children in the production process monitoring of the syrup for treating the common cold of the children is provided.
According to another aspect of the invention, a method for detecting the quality of the syrup for treating common cold and fever in children is provided. The method comprises the following steps: preparing chromatographic peaks of a sample to be detected; comparing the chromatographic peak of the sample to be detected with the fingerprint of the syrup for treating the common cold and fever of the children, and if the similarity is greater than 0.9, indicating that the sample to be detected is qualified.
By applying the technical scheme of the invention, 18 common peaks are generated by the fingerprint characteristic spectrum of the syrup (main components of isatis root, weeping forsythia, dyers woad leaf, mulberry twig, fineleaf schizonepeta herb, divaricate saposhnikovia root and perilla leaf), so that rich identification information can be provided, the types and the amounts of chemical components contained in the syrup for treating the common cold of the children can be comprehensively reflected, and the quality of the syrup is integrally described and evaluated.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 shows chromatograms of a pediatric cold defervescence syrup sample and 7 negative samples;
FIG. 2 shows chromatograms of pediatric cold antipyretic syrup samples and 5 controls ((R, S) goiter, cimicifugain, 5-O-methylvisamiloride, forsythin, indirubin);
FIG. 3 shows a chromatogram of a sample of 10 batches of pediatric cold antipyretic syrup and a control chromatogram; and
fig. 4 shows a control fingerprint: peak 3: (R, S-epigoitrin), peak 8: cimicifugatin, peak 14: 5-O-methyl-vidamiloride, peak 17 (S): forsythin, peak 18: indirubin.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The invention will be described in detail below with reference to the drawings in connection with embodiments.
According to an exemplary embodiment of the invention, a method for establishing a fingerprint spectrum of syrup for treating common cold and fever in children is provided. The establishing method comprises the following steps: 1) Preparing a sample solution and a reference solution; 2) Sample injection analysis is respectively carried out on the sample solution and the reference solution by adopting HPLC, so as to obtain the HPLC fingerprint of the sample solution; 3) And (3) introducing the HPLC fingerprint data of the sample solution into 2012 edition of a traditional Chinese medicine fingerprint similarity evaluation system, taking 1 fingerprint of the sample solution as a reference spectrum, and generating a pediatric cold antipyretic syrup fingerprint reference spectrum by an average method.
By applying the technical scheme of the invention, 18 common peaks are generated by the fingerprint characteristic spectrum of the syrup (main components of isatis root, weeping forsythia, dyers woad leaf, mulberry twig, fineleaf schizonepeta herb, divaricate saposhnikovia root and perilla leaf), so that rich identification information can be provided, the types and the amounts of chemical components contained in the syrup for treating the common cold of the children can be comprehensively reflected, and the quality of the syrup is integrally described and evaluated.
In order to obtain a more accurate fingerprint, preparing a test solution includes: weighing 5mL of the antipyretic syrup for treating the common cold of the children, placing in a 50mL volumetric flask, adding methanol, performing ultrasonic treatment for 30min, standing to a 50mL scale after reaching room temperature, shaking uniformly, filtering with a 0.45 μm microporous filter membrane, and taking the subsequent filtrate. Preferably, preparing the reference solution comprises: placing the forsythin reference substance into a volumetric flask, adding methanol to obtain solution containing 0.1mg of forsythin per 1mL, filtering with 0.45 μm microporous membrane, and collecting the filtrate.
Preferably, step 2) specifically includes: taking the same batch of sample solution of the syrup for treating common cold and fever of children, continuously injecting the sample for 6 times, and recording a chromatogram; taking the same batch of sample solutions of the infant cold antipyretic syrup, respectively injecting at 0,2,4,8 and 16 hours, and recording a chromatogram; simultaneously preparing N parts of sample solutions of the infant cold antipyretic syrup, respectively injecting samples, recording a chromatogram, wherein N is more than or equal to 6, for example, N=6.
In a preferred embodiment of the invention, HPLC is carried out using a Agilent ZORBAX SB-C18 chromatographic column, 250mm by 4.6mm,5 μm; acetonitrile is taken as a mobile phase A, 0.1% phosphoric acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specifications in the following table;
the detection wavelength is 277nm; the column temperature is 30 ℃; the flow rate is 1.0ml per minute, the theoretical plate number is not less than 3000 calculated according to the forsythin peak, and the chromatographic peak obtained under the condition is obviously superior to other elution systems.
Typically, the main components of the syrup for treating common cold and fever of children include: radix Isatidis, fructus forsythiae, folium Isatidis, ramulus Mori, herba Schizonepetae, radix Saposhnikoviae, and folium Perillae; preferably, the fingerprint of the antipyretic syrup for children in step 2) has 18 common chromatographic peaks, wherein the 18 peaks are respectively a peak 1 with a relative retention time of 0.128, a peak 2 with a relative retention time of 0.166, a peak 3 with a relative retention time of 0.201, a peak 4 with a relative retention time of 0.219, a peak 5 with a relative retention time of 0.230, a peak 6 with a relative retention time of 0.250, a peak 7 with a relative retention time of 0.290, a peak 8 with a relative retention time of 0.382, a peak 9 with a relative retention time of 0.508, a peak 10 with a relative retention time of 0.609, a peak 11 with a relative retention time of 0.634, a peak 12 with a relative retention time of 0.667, a peak 13 with a relative retention time of 0.717, a peak 14 with a relative retention time of 0.761, a peak 15 with a relative retention time of 0.916, a peak 16 with a relative retention time of 0.984, a peak with a relative retention time of 0.100, and a peak 18 with a relative retention time of 1.100.
According to another aspect of the invention, a child cold antipyretic syrup fingerprint obtained by the construction method of the child cold antipyretic syrup fingerprint is provided.
Further, it includes a peak No. 1 with a relative retention time of 0.128, a peak No. 2 with a relative retention time of 0.166, a peak No. 3 with a relative retention time of 0.201, a peak No. 4 with a relative retention time of 0.219, a peak No. 5 with a relative retention time of 0.230, a peak No. 6 with a relative retention time of 0.250, a peak No. 7 with a relative retention time of 0.290, a peak No. 8 with a relative retention time of 0.382, a peak No. 9 with a relative retention time of 0.508, a peak No. 10 with a relative retention time of 0.609, a peak No. 11 with a relative retention time of 0.634, a peak No. 12 with a relative retention time of 0.667, a peak No. 13 with a relative retention time of 0.717, a peak No. 14 with a relative retention time of 0.761, a peak No. 15 with a relative retention time of 0.916, a peak No. 16 with a relative retention time of 0.984, a peak No. 17 with a relative retention time of 0.100, and a peak No. 18 with a relative retention time of 1.376.
According to still another aspect of the invention, the application of the fingerprint spectrum of the syrup for treating the common cold of the children in the production process monitoring of the syrup for treating the common cold of the children is provided.
According to another aspect of the invention, a method for detecting the quality of the syrup for treating common cold and fever in children is provided. The method comprises the following steps: preparing chromatographic peaks of a sample to be detected; comparing the chromatographic peak of the sample to be detected with the fingerprint of the syrup for treating the common cold and fever of the children, and if the similarity is greater than 0.9, indicating that the sample to be detected is qualified. By applying the technical scheme of the invention, 18 common peaks are generated by the fingerprint characteristic spectrum of the syrup (main components of isatis root, weeping forsythia, dyers woad leaf, mulberry twig, fineleaf schizonepeta herb, divaricate saposhnikovia root and perilla leaf), so that rich identification information can be provided, the types and the amounts of chemical components contained in the syrup for treating the common cold of the children can be comprehensively reflected, and the quality of the syrup is integrally described and evaluated.
The advantageous effects of the present invention will be further described below with reference to examples.
Example 1
HPLC fingerprint method for syrup for treating common cold and fever in children
1. Chromatographic condition and System applicability test
A Agilent ZORBAX SB-C18 column (250 mm. Times.4.6 mm,5 μm) was used; acetonitrile as mobile phase a and 0.1% phosphoric acid solution as mobile phase B, and gradient elution was performed as specified in table 1 below; the detection wavelength is 277nm; the column temperature is 30 ℃; the flow rate was 1.0ml per minute. The theoretical plate number is not less than 3000 calculated according to the forsythin peak.
TABLE 1
2. Preparation of reference solutions
Taking a proper amount of a forsythin (batch number: 110821-202117, content of which is 94.9%) reference substance, precisely weighing, placing into a volumetric flask, adding methanol to prepare a solution containing 0.1mg of forsythin per 1mL, filtering with a 0.45 μm microporous filter membrane, and collecting the subsequent filtrate.
3. Preparation of test solutions
Precisely weighing 5mL of the antipyretic syrup for treating infantile common cold, placing in a 50mL volumetric flask, adding appropriate amount of methanol, performing ultrasonic treatment for 30min, standing to scale after reaching room temperature, shaking, filtering with 0.45 μm microporous membrane, and collecting the subsequent filtrate.
4. Methodology investigation
4.1 examining the precision, taking the same batch of infant cold antipyretic syrup test sample solution, continuously injecting the sample for 6 times, recording the chromatogram, wherein the relative retention time of each common peak is less than 3% in the result, and the relative peak area is less than 5% in the result, which indicates that the instrument precision is better. The results are shown in tables 2 and 3.
TABLE 2
TABLE 3 Table 3
4.2 stability investigation the same batch of infant cold antipyretic syrup test samples are taken, sample injection is carried out at 0,2,4,8 and 16 hours respectively, a chromatogram is recorded, and the relative retention time of each common peak has RSD of <3 percent and the relative peak area has RSD of <5 percent, which indicates that the test sample solution has good stability within 16 hours. The results are shown in tables 4 and 5.
TABLE 4 Table 4
TABLE 5
4.3 repeatability investigation 6 parts of infant cold antipyretic syrup test sample solutions are prepared simultaneously, sample injection is carried out respectively, a chromatogram is recorded, and the relative retention time of each common peak is less than 3% and the relative peak area is less than 5%, so that the method has better repeatability. The results are shown in Table 6 and Table 7.
TABLE 6
TABLE 7
5. Fingerprint establishment and similarity analysis
Taking 10 batches (S1-S10) of the syrup for treating the common cold and the reference substance, preparing the syrup according to the method (namely taking 5mL of the syrup or the reference substance for treating the common cold and precisely measuring the syrup or the reference substance for treating the common cold and placing the syrup or the reference substance into a 50mL volumetric flask, adding a proper amount of methanol, performing ultrasonic treatment for 30min, standing to reach a scale after the room temperature, shaking uniformly, filtering by using a microporous filter membrane with the size of 0.45 mu m, taking the subsequent filtrate, precisely sucking 10 mu L of each of the reference substance solution and the sample solution, injecting the reference substance solution and the sample solution into a liquid chromatograph, and measuring according to the chromatographic conditions. The evaluation is carried out by adopting a traditional Chinese medicine fingerprint similarity evaluation system (2012.0 edition), S1 is used as a reference spectrum in the figure 3, a control spectrum R is generated, 18 common peaks are shown in the figure 4, wherein 17 peaks are forsythin (reference peak), and the similarity of the common cold antipyretic syrup of each batch of children and the control fingerprint is 0.9-1.0, as shown in the table 8.
TABLE 8
6. Investigation of specificity
According to the preparation method of the test sample (precisely measuring 5mL of the infant cold antipyretic syrup, placing the infant cold antipyretic syrup in a 50mL volumetric flask, adding a proper amount of methanol, carrying out ultrasonic treatment for 30min, carrying out constant volume to scale after the temperature reaches the room temperature, shaking the infant cold antipyretic syrup to be uniform, filtering the infant cold antipyretic syrup by using a microporous filter membrane with the size of 0.45 mu m, taking the subsequent filtrate to obtain the infant cold antipyretic syrup, simultaneously preparing 7 medicinal material negative test samples, the infant cold antipyretic syrup solution ((R, S) and the reference solution (with the content of 100.0% in batch number: 111753-202007), the content of cimicifugal glycoside (with the content of 94.6% in batch number: 111522-201613), the content of 5-O-methylvismin glycoside (with the content of 97.4% in batch number: 110821-202117) and the content of indigomonas (with the content of 99.1%), respectively recording chromatograms, and determining the attribution of each characteristic peak according to the obtained batch maps. The results are shown in FIGS. 1 and 2, table 9.
TABLE 9
In summary, it can be seen that the 18 common peaks provided by the method of the present application respectively belong to 7 medicinal materials of the syrup for treating the common cold of children, and comprehensively reflect the distribution and the proportion relation of various components of the syrup for treating the common cold of children.
Therefore, the method of the invention has the advantages of simple operation and large information quantity compared with the method of directly detecting several chemicals in the preparation by comparing and analyzing various components in the 7 medicinal materials of the syrup for treating the common cold and reducing fever of children, and can comprehensively control the quality of the syrup for treating the common cold and reducing fever of children.
From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects: the fingerprint characteristic spectrum of the syrup for treating the common cold of the children (main components of isatis root, weeping forsythia, dyers woad leaf, mulberry twig, fineleaf schizonepeta herb, divaricate saposhnikovia root and perilla leaf) generates 18 common peaks, can provide rich identification information, can more comprehensively reflect the types and the amounts of chemical components contained in the syrup for treating the common cold of the children, and further integrally describes and evaluates the quality of the syrup.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The method for establishing the fingerprint of the syrup for treating the common cold and fever of the children is characterized by comprising the following steps of:
1) Preparing a sample solution and a reference solution;
2) Carrying out sample injection analysis on the sample solution and the reference solution by adopting HPLC (high performance liquid chromatography) to obtain an HPLC fingerprint of the sample solution;
3) Introducing the HPLC fingerprint data of the sample solution into 2012 version of a traditional Chinese medicine fingerprint similarity evaluation system, taking 1 fingerprint of the sample solution as a reference fingerprint, and generating a pediatric cold antipyretic syrup fingerprint reference fingerprint by an average method;
the preparation of the test solution comprises: weighing 5mL of the syrup for treating the common cold of the children, placing the syrup in a 50mL volumetric flask, adding methanol, carrying out ultrasonic treatment for 30min, standing to a 50mL scale after reaching room temperature, shaking uniformly, filtering with a 0.45 mu m microporous filter membrane, and taking a subsequent filtrate to obtain the syrup;
the preparation of the reference solution comprises: placing the forsythin reference substance into a volumetric flask, adding methanol to prepare a solution containing 0.1mg of forsythin per 1mL, filtering with a 0.45 μm microporous filter membrane, and collecting the subsequent filtrate;
the step 2) specifically comprises the following steps:
simultaneously preparing N parts of sample solutions of the infant cold antipyretic syrup, respectively injecting samples, and recording chromatograms, wherein N is more than or equal to 6;
HPLC is carried out on Agilent ZORBAX SB-C18 chromatographic column with the specification of 250mm×4.6mm and 5 μm; acetonitrile is taken as a mobile phase A, 0.1% phosphoric acid solution is taken as a mobile phase B, and gradient elution is carried out according to the specifications in the following table;
；
the detection wavelength is 277nm; the column temperature is 30 ℃; the flow rate is 1.0ml per minute, and the theoretical plate number is not less than 3000 calculated according to the forsythin peak;
the main components of the syrup for treating the common cold and reducing fever of the children comprise: radix Isatidis, fructus forsythiae, folium Isatidis, ramulus Mori, herba Schizonepetae, radix Saposhnikoviae, and folium Perillae;
the fingerprint of the infant cold antipyretic syrup in step 2) is confirmed to have 18 common chromatographic peaks, wherein the 18 common chromatographic peaks are respectively a peak 1 with a relative retention time of 0.128, a peak 2 with a relative retention time of 0.166, a peak 3 with a relative retention time of 0.201, a peak 4 with a relative retention time of 0.219, a peak 5 with a relative retention time of 0.230, a peak 6 with a relative retention time of 0.250, a peak 7 with a relative retention time of 0.290, a peak 8 with a relative retention time of 0.382, a peak 9 with a relative retention time of 0.508, a peak 10 with a relative retention time of 0.609, a peak 11 with a relative retention time of 0.634, a peak 12 with a relative retention time of 0.667, a peak 13 with a relative retention time of 0.717, a peak 14 with a relative retention time of 0.761, a peak 15 with a relative retention time of 0.916, a peak 16 with a relative retention time of 0.984, a peak with a relative retention time of 0.376, and a peak with a retention time of 1.376.
2. The method of claim 1, further comprising a precision investigation and a stability investigation, the precision investigation comprising: taking the same batch of sample solution of the syrup for treating common cold and fever of children, continuously injecting the sample for 6 times, and recording a chromatogram;
the stability study includes: taking the same batch of sample solutions of the syrup for treating common cold and fever of children, respectively injecting at 0,2,4,8 and 16h, and recording the chromatogram.
3. The use of the pediatric cold antipyretic syrup fingerprint obtained by the construction method of the pediatric cold antipyretic syrup fingerprint according to any one of claims 1 to 2 in monitoring the pediatric cold antipyretic syrup production process.
4. The quality detection method of the syrup for treating the common cold and fever of the children is characterized by comprising the following steps of:
preparing chromatographic peaks of a sample to be detected;
comparing the chromatographic peak of the sample to be detected with the fingerprint of the infant cold antipyretic syrup obtained by the construction method of the fingerprint of the infant cold antipyretic syrup in any one of claims 1 to 2, and if the similarity is more than 0.9, indicating that the sample to be detected is qualified.
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