CN108195988B - Schisandra chinensis medicinal material adopting HPLC fingerprint construction method and pulse activating injection preparation thereof - Google Patents
Schisandra chinensis medicinal material adopting HPLC fingerprint construction method and pulse activating injection preparation thereof Download PDFInfo
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- CN108195988B CN108195988B CN201810099906.1A CN201810099906A CN108195988B CN 108195988 B CN108195988 B CN 108195988B CN 201810099906 A CN201810099906 A CN 201810099906A CN 108195988 B CN108195988 B CN 108195988B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 114
- 239000000463 material Substances 0.000 title claims abstract description 103
- 240000006079 Schisandra chinensis Species 0.000 title claims abstract description 93
- 235000008422 Schisandra chinensis Nutrition 0.000 title claims abstract description 92
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 92
- 238000002347 injection Methods 0.000 title claims abstract description 89
- 239000007924 injection Substances 0.000 title claims abstract description 89
- 238000010276 construction Methods 0.000 title claims abstract description 15
- 230000003213 activating effect Effects 0.000 title claims abstract description 9
- 239000012085 test solution Substances 0.000 claims abstract description 27
- 238000004458 analytical method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 238000001228 spectrum Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- YEFOAORQXAOVJQ-RZFZLAGVSA-N schisandrol a Chemical compound C1[C@H](C)[C@@](C)(O)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC YEFOAORQXAOVJQ-RZFZLAGVSA-N 0.000 claims description 36
- YEFOAORQXAOVJQ-UHFFFAOYSA-N wuweizischun A Natural products C1C(C)C(C)(O)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC YEFOAORQXAOVJQ-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 26
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- 239000009877 shengmai Substances 0.000 claims description 18
- 239000013558 reference substance Substances 0.000 claims description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000010828 elution Methods 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000012088 reference solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003643 water by type Substances 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000004811 liquid chromatography Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000008213 purified water Substances 0.000 claims description 4
- 238000003908 quality control method Methods 0.000 abstract description 5
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 4
- 230000014759 maintenance of location Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OIRDTQYFTABQOQ-KQYNXXCUSA-N adenosine Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O OIRDTQYFTABQOQ-KQYNXXCUSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035900 sweating Effects 0.000 description 2
- 239000002126 C01EB10 - Adenosine Substances 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 241000218377 Magnoliaceae Species 0.000 description 1
- 240000002948 Ophiopogon intermedius Species 0.000 description 1
- 206010033557 Palpitations Diseases 0.000 description 1
- 235000002789 Panax ginseng Nutrition 0.000 description 1
- 229960005305 adenosine Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 206010007625 cardiogenic shock Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 208000016253 exhaustion Diseases 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002458 infectious effect Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000010255 intramuscular injection Methods 0.000 description 1
- 239000007927 intramuscular injection Substances 0.000 description 1
- 238000001990 intravenous administration Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 208000010125 myocardial infarction Diseases 0.000 description 1
- 239000002777 nucleoside Substances 0.000 description 1
- 150000003833 nucleoside derivatives Chemical class 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- JXOHGGNKMLTUBP-HSUXUTPPSA-N shikimic acid Chemical compound O[C@@H]1CC(C(O)=O)=C[C@@H](O)[C@H]1O JXOHGGNKMLTUBP-HSUXUTPPSA-N 0.000 description 1
- JXOHGGNKMLTUBP-JKUQZMGJSA-N shikimic acid Natural products O[C@@H]1CC(C(O)=O)=C[C@H](O)[C@@H]1O JXOHGGNKMLTUBP-JKUQZMGJSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 208000013220 shortness of breath Diseases 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a schisandra chinensis medicinal material and a pulse activating injection preparation thereof by adopting a construction method of an HPLC fingerprint, and relates to the field of detection of traditional Chinese medicines and preparations. The method comprises the steps of injecting a test solution of a schisandra chinensis medicinal material or a pulse-activating injection preparation test solution into a liquid chromatograph for high performance liquid chromatography analysis to obtain an HPLC fingerprint of the schisandra chinensis medicinal material or an HPLC fingerprint of the pulse-activating injection preparation, and establishing an analysis method of the schisandra chinensis medicinal material and the pulse-activating injection preparation for evaluating the correlation of the medicinal materials and the preparation and realizing the quality control from the medicinal materials to the preparation; by establishing HPLC fingerprint spectra of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof, the relative contents of main components in the schisandra chinensis medicinal material and the preparation thereof are accurately analyzed and measured, and the product quality can be effectively and reliably predicted according to the contents, so that the quality of the medicinal material and the correlation between the medicinal material and the preparation can be comprehensively evaluated.
Description
Technical Field
The invention relates to the field of detection of traditional Chinese medicines and preparations, and in particular relates to a schisandra chinensis medicinal material and a pulse-activating injection preparation thereof, which adopt a construction method of an HPLC fingerprint.
Background
Fructus Schisandrae chinensis is dried mature fruit of Schisandra chinensis (Turcz.) Baill of Magnoliaceae, and has effects of astringing lung, relieving cough, nourishing, arresting seminal emission, relieving diarrhea, and arresting sweating. The pulse-activating injection is a traditional Chinese medicine preparation prepared from red ginseng, dwarf lilyturf tuber and Chinese magnoliavine fruit, can be administrated by adopting an intramuscular injection or intravenous drip mode, and is used for treating palpitation, shortness of breath, cold limbs, sweating, pulse exhaustion, myocardial infarction, cardiogenic shock, infectious shock and the like with the symptoms of deficiency of both qi and yin and pulse deficiency and collapse. The schisandra chinensis and the pulse-activating injection are clinically used for many years, and the quality condition of the schisandra chinensis and the pulse-activating injection cannot be comprehensively reflected only by controlling the content of schizandrol A in the Chinese pharmacopoeia at the present stage.
The fingerprint is a technology for integrally researching a complex substance system, is developed along with the development of modern analysis technology, is applied to the fields of environmental protection, food evaluation, quality control of traditional Chinese medicines and the like at present, and is widely applied to traditional Chinese medicines in particular. The traditional Chinese medicine fingerprint spectrum refers to the spectrum or spectrum of a certain kind or several kinds of components which are common in a certain traditional Chinese medicine and a preparation thereof and have characteristics. Although the establishment of the fingerprint has a very important significance for effectively controlling the quality of the schisandra and the preparation thereof, at present, no establishment method of the fingerprint of the schisandra medicinal material and the pulse-activating injection preparation thereof exists, so that the purpose of comprehensively evaluating the quality of the schisandra medicinal material and the preparation thereof cannot be achieved without establishing the fingerprint of the schisandra medicinal material and the pulse-activating injection preparation thereof.
Therefore, the construction method of the fingerprint of the schisandra chinensis medicinal material and the pulse-activating infusion preparation thereof needs to be researched.
Disclosure of Invention
The invention aims to provide a method for constructing a High Performance Liquid Chromatography (HPLC) fingerprint of a schisandra chinensis medicinal material and a pulse-activating injection preparation thereof, establishes an analysis method of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof, is used for evaluating the correlation of the medicinal materials and the preparation, and realizes the quality control from the medicinal materials to the preparation.
The invention also aims to provide application of the HPLC fingerprint of the schisandra chinensis and the pulse-activating injection preparation thereof, wherein the HPLC fingerprint of the schisandra chinensis and the pulse-activating injection preparation thereof is established, so that the relative contents of main components in the schisandra chinensis and the preparation thereof are accurately analyzed and determined, and the product quality can be effectively and reliably predicted according to the contents, thereby comprehensively evaluating the quality of the medicinal materials and the correlation between the medicinal materials and the preparation.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a method for constructing an HPLC fingerprint of a schisandra chinensis medicinal material and a pulse-activating injection preparation thereof, which comprises the following steps of injecting a schisandra chinensis medicinal material test solution or a pulse-activating injection preparation test solution into a liquid chromatograph for high performance liquid chromatography analysis to obtain the HPLC fingerprint of the schisandra chinensis medicinal material or the HPLC fingerprint of the pulse-activating injection preparation, wherein the conditions of the liquid chromatography are as follows: waters symmetry shieldTMRP18A chromatographic column; the detection wavelength is 250-260 nm, and the flow rate of the mobile phase is 0.8-1.3 mL·min-1The column temperature is 26-40 ℃; the mobile phase A is acetonitrile, the mobile phase B is phosphoric acid water solution with the volume percentage of 0.02-0.04%, and the mobile phase A and the mobile phase B adopt gradient elution.
Further, in the preferred embodiment of the present invention, the Waters symmetry shieldTMRP18The size of the column was 4.6mm × 250mm, 5.0 μm.
Further, in a preferred embodiment of the present invention, the gradient elution requirement is as follows, wherein the ratio between mobile phase a and mobile phase B is volume ratio:
at 0min, mobile phase a: mobile phase B ═ 0: 100, respectively;
at 17min, mobile phase a: mobile phase B ═ 4: 96;
at 20min, mobile phase a: mobile phase B ═ 10: 90, respectively;
at 40min, mobile phase a: mobile phase B15: 85 parts by weight;
at 60min, mobile phase a: mobile phase B60: 40;
at 70min, mobile phase a: mobile phase B95: 5;
at 75min, mobile phase a: mobile phase B95: 5;
at 80min, mobile phase a: mobile phase B ═ 0: 100.
further, in a preferred embodiment of the present invention, the preparation method of the schisandra chinensis medicinal material test solution comprises: weighing fructus Schisandrae, adding purified water, decocting, filtering, and collecting filtrate as fructus Schisandrae test solution; the pulse activating injection preparation test solution is prepared according to the pulse activating injection preparation process.
Further, in a preferred embodiment of the present invention, the schizandrol A reference substance solution is absorbed and injected into a liquid chromatograph for high performance liquid chromatography analysis, so as to obtain the HPLC fingerprint of the schizandrol A reference substance solution, wherein the conditions of the liquid chromatography are as follows: waters symmetry shieldTMRP18A chromatographic column; the detection wavelength is 250-260 nm, and the flow rate of the mobile phase is 0.8-1.3 mL/min-1The column temperature is 26-40 ℃; the mobile phase A is acetonitrile, and the mobile phase B is phosphoric acid water solution with the volume percentage of 0.02 percent to 0.04 percentAnd the mobile phase A and the mobile phase B adopt gradient elution.
Further, in a preferred embodiment of the present invention, the preparation method of the schizandrol A reference solution comprises: weighing the schizandrol A, adding methanol and mixing to obtain a schizandrol A reference substance solution, wherein the content of the schizandrol A in the schizandrol A reference substance solution is 8-13 mu g/ml.
The application of the construction method of the HPLC fingerprint of the schisandra chinensis medicinal material and the Shengmai injection preparation thereof is used for comprehensively evaluating the correlation between the schisandra chinensis medicinal material and the Shengmai injection preparation by comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material and the HPLC fingerprint of the Shengmai injection preparation.
Further, in the preferred embodiment of the invention, the HPLC fingerprint of the schisandra chinensis medicinal material and the HPLC fingerprint of the pulse-activating injection preparation are analyzed, and the relative retention time and the relative peak area of the characteristic peak in the schisandra chinensis medicinal material and the pulse-activating injection preparation are respectively obtained by taking the schizandrol A as a reference peak;
the corresponding characteristic peak between the schisandra chinensis medicinal material and the pulse-activating injection preparation is obtained by comparing the relative retention time and the relative peak area of the characteristic peak of the schisandra chinensis medicinal material and the relative retention time and the relative peak area of the characteristic peak of the pulse-activating injection preparation, so that the correlation between the schisandra chinensis medicinal material and the pulse-activating injection preparation is obtained.
The application of the HPLC fingerprints of the schisandra chinensis medicinal material and the Shengmai injection preparation thereof is used for measuring the relative content of main components in the schisandra chinensis medicinal material or the Shengmai injection preparation by comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material or the HPLC fingerprint of the Shengmai injection preparation and the HPLC fingerprint of a schizandrol A reference substance solution.
Furthermore, in the preferred embodiment of the present invention, the relative content of the main ingredient in the schisandra chinensis medicinal material or the pulse-activating injection preparation is obtained by comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material or the HPLC fingerprint of the pulse-activating injection preparation with the characteristic peak in the HPLC fingerprint of the schizandrol A control solution.
Application of the embodiments of the present inventionThe schisandra chinensis medicinal material and the pulse-activating injection preparation of the construction method of the HPLC fingerprint have the beneficial effects that: the method for constructing the HPLC fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof comprises the following steps of injecting a schisandra chinensis medicinal material test solution or a pulse-activating injection preparation test solution into a liquid chromatograph for high performance liquid chromatography analysis, thus obtaining the HPLC fingerprint of the schisandra chinensis medicinal material or the pulse-activating injection preparation, wherein the conditions of the liquid chromatography are as follows: waters symmetry shieldTMRP18A chromatographic column; the detection wavelength is 250-260 nm, and the flow rate of the mobile phase is 0.8-1.3 mL/min-1The column temperature is 26-40 ℃; the mobile phase A is acetonitrile, the mobile phase B is phosphoric acid aqueous solution with the volume percentage of 0.02-0.04%, the mobile phase A and the mobile phase B adopt gradient elution, and the method for constructing the high performance liquid chromatography fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation establishes the analysis method of the schisandra chinensis medicinal material and the pulse-activating injection preparation, is used for evaluating the correlation of the medicinal material and the preparation, and realizes the quality control from the medicinal material to the preparation; by establishing HPLC fingerprint spectra of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof, the relative contents of main components in the schisandra chinensis medicinal material and the preparation thereof are accurately analyzed and measured, and the product quality can be effectively and reliably predicted according to the contents, so that the quality of the medicinal material and the correlation between the medicinal material and the preparation can be comprehensively evaluated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an HPLC fingerprint of Schisandra chinensis medicinal material in example 1 of the present invention;
fig. 2 is an HPLC fingerprint of the pulse-activating injection preparation of example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The schisandra chinensis medicinal material and the pulse-activating injection preparation thereof adopting the construction method of the HPLC fingerprint spectrum of the embodiment of the invention are specifically explained below.
The embodiment of the invention provides a method for constructing an HPLC fingerprint of a schisandra chinensis medicinal material and a pulse-activating injection preparation thereof, which is used for analyzing and constructing a schisandra chinensis medicinal material test sample solution or a pulse-activating injection preparation test sample by utilizing high performance liquid chromatography. The specific method comprises the following steps:
(1) obtaining a test solution: a. preparing a schisandra chinensis medicinal material test solution: weighing fructus Schisandrae, adding purified water, decocting, filtering, and collecting filtrate as fructus Schisandrae test solution; b. the preparation test solution is obtained according to the production process of the pulse-activating injection and is used as the pulse-activating injection preparation test solution.
(2) Obtaining a reference solution: weighing the schizandrol A, adding methanol and mixing to obtain a schizandrol A reference substance solution, wherein the content of the schizandrol A in the schizandrol A reference substance solution is 8-13 (10) mu g/ml.
(3) Constructing a fingerprint of a test sample: sucking the schizandrol A reference substance solution, injecting into a liquid chromatograph for high performance liquid chromatography analysis to obtain the HPLC fingerprint of the schizandrol A reference substance solution, wherein the conditions of the liquid chromatography are as follows: waters symmetry shieldTMRP18A chromatographic column with specification of 4.6mm × 250mm and 5.0 μm, detection wavelength of 250-260 (254) nm, and flow rate of mobile phase of 0.8-1.3 (1.0) mL/min-1The column temperature is 26-40 (30) DEG C; the mobile phase a is acetonitrile, the mobile phase B is a phosphoric acid aqueous solution with a volume percentage of 0.02% -0.04% (0.03%), and the mobile phase a and the mobile phase B are subjected to gradient elution, in this embodiment, the gradient elution is required as follows, wherein the ratio of the mobile phase a to the mobile phase B is a volume ratio:
at 0min, mobile phase a: mobile phase B ═ 0: 100, respectively;
at 17min, mobile phase a: mobile phase B ═ 4: 96;
at 20min, mobile phase a: mobile phase B ═ 10: 90, respectively;
at 40min, mobile phase a: mobile phase B15: 85 parts by weight;
at 60min, mobile phase a: mobile phase B60: 40;
at 70min, mobile phase a: mobile phase B95: 5;
at 75min, mobile phase a: mobile phase B95: 5;
at 80min, mobile phase a: mobile phase B ═ 0: 100.
(4) constructing a fingerprint of a reference substance: injecting the test solution of the schisandra chinensis medicinal material or the pulse-activating injection preparation test solution into a liquid chromatograph for high performance liquid chromatography analysis to obtain the HPLC fingerprint of the schisandra chinensis medicinal material or the HPLC fingerprint of the pulse-activating injection preparation, wherein the conditions of the liquid chromatography are as follows: waters symmetry shieldTMRP18A chromatographic column with specification of 4.6mm × 250mm and 5.0 μm, detection wavelength of 250-260 (254) nm, and flow rate of mobile phase of 0.8-1.3 (1.0) mL/min-1The column temperature is 26-40 (30) DEG C; the mobile phase A is acetonitrile, the mobile phase B is phosphoric acid water solution with the volume percentage of 0.02 percent to 0.04 percent (0.03 percent), the mobile phase A and the mobile phase B adopt gradient elution, and the gradient elution requirement is the same as the gradient elution requirement.
The embodiment of the invention also provides an application of the construction method of the HPLC fingerprint of the schisandra chinensis medicinal material and the Shengmai injection preparation thereof, and the correlation between the schisandra chinensis medicinal material and the Shengmai injection preparation is comprehensively evaluated by comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material and the HPLC fingerprint of the Shengmai injection preparation.
The specific process is as follows: analyzing the HPLC fingerprint of the schisandra chinensis medicinal material and the HPLC fingerprint of the pulse-activating injection preparation, and respectively obtaining the relative retention time and the relative peak area of the characteristic peak in the schisandra chinensis medicinal material and the pulse-activating injection preparation by taking schisandrin as a reference peak;
obtaining the corresponding characteristic peak between the schisandra chinensis medicinal material and the pulse-activating injection preparation by comparing the relative retention time and the relative peak area of the characteristic peak of the schisandra chinensis medicinal material and the relative retention time and the relative peak area of the characteristic peak of the pulse-activating injection preparation;
the embodiment of the invention also provides an application of the HPLC fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof, and the application is used for determining the relative content of main components in the schisandra chinensis medicinal material or the pulse-activating injection preparation by comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material or the HPLC fingerprint of the pulse-activating injection preparation and the HPLC fingerprint of a schizandrol A reference substance solution.
The specific process is as follows: and comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material or the HPLC fingerprint of the shengmai injection preparation with the characteristic peak in the HPLC fingerprint of the schizandrol A reference substance solution to obtain the relative content of the main components in the schisandra chinensis medicinal material or the shengmai injection preparation.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
firstly, precisely weighing 2g of schisandra chinensis, adding 100ml of purified water, decocting for 2 hours, filtering, and collecting a subsequent filtrate as a test solution of a medicinal material; the preparation test solution is obtained according to the production process of the pulse-activating injection.
Secondly, weighing the schizandrol A, adding methanol and mixing to obtain a reference solution, wherein the content of the schizandrol A in the reference solution is 10 mu g/ml.
Step three, facilitating HPLC to determine the chromatographic conditions of the medicinal material test solution or the preparation test solution: waterssymetry shieldTMRP18Chromatographic column of 4.6mm × 250mm and 5.0 μm, detection wavelength of 254nm, and flow rate of mobile phase of 1.0 mL/min-1The column temperature is 30 ℃; the mobile phase A is acetonitrile, the mobile phase B is 0.03 percent phosphoric acid water solution by volume percentage, and the mobile phases A and B adopt gradient elution, wherein the gradient elution is requiredThe following is solved, wherein the ratio between the mobile phase A and the mobile phase B is volume ratio:
at 0min, mobile phase a: mobile phase B ═ 0: 100, respectively;
at 17min, mobile phase a: mobile phase B ═ 4: 96;
at 20min, mobile phase a: mobile phase B ═ 10: 90, respectively;
at 40min, mobile phase a: mobile phase B15: 85 parts by weight;
at 60min, mobile phase a: mobile phase B60: 40;
at 70min, mobile phase a: mobile phase B95: 5;
at 75min, mobile phase a: mobile phase B95: 5;
at 80min, mobile phase a: mobile phase B ═ 0: 100.
precisely absorbing 10 mu l of sample volume of the test solution of the medicinal material or the preparation test solution under the chromatographic conditions, and carrying out high performance liquid chromatography analysis to obtain the HPLC fingerprint of the schisandra chinensis medicinal material and the HPLC fingerprint of the Shengmai injection preparation.
Fourthly, facilitating HPLC to determine the chromatographic conditions of the reference solution: waters symmetry shieldTMRP18Chromatographic column of 4.6mm × 250mm and 5.0 μm, detection wavelength of 254nm, and flow rate of mobile phase of 1.0 mL/min-1The column temperature is 30 ℃; the mobile phase A is acetonitrile, the mobile phase B is 0.03 percent phosphoric acid water solution by volume percentage, and the mobile phases A and B adopt gradient elution.
And precisely sucking 10 mu l of sample volume of the reference substance solution under the chromatographic conditions, and performing high performance liquid chromatography to obtain the HPLC fingerprint of the reference substance solution.
The HPLC fingerprint of the schisandra chinensis medicinal material, the HPLC fingerprint of the shengmai injection preparation and the HPLC fingerprint of the reference solution are obtained through the construction process, wherein the HPLC fingerprint of the schisandra chinensis medicinal material is shown in figure 1, and the HPLC fingerprint of the shengmai injection preparation is shown in figure 2. According to the HPLC fingerprint of the schisandra chinensis medicinal material, the HPLC fingerprint of the Shengmai injection preparation and the HPLC fingerprint of the reference substance solution, the following analysis is carried out:
A. in the HPLC fingerprint spectrum of the schisandra chinensis medicinal material, the total number of 24 characteristic peaks is marked by integrating 5 percent of the area of the schizandrol A peak, wherein 5 characteristic peaks are identified as follows: peak #3 is shikimic acid, peak #6 is nucleoside, peak #7 is adenosine, peak #9 is pentamethyl furfural, and peak #23 is schizandrol A.
In the HPLC fingerprint spectrum of the schisandra chinensis medicinal material, the schisandrin is taken as a reference peak, and the relative retention time of 24 characteristic peaks is respectively as follows: 0.050 to 0.055(#1), 0.063 to 0.068(#2), 0.078 to 0.083(#3), 0.090 to 0.095(#4), 0.08 to 0.13(#5), 0.13 to 0.18(#6), 0.14 to 0.19(#7), 0.23 to 0.28(#8), 0.27 to 0.32(#9), 0.32 to 0.37(#10), 0.36 to 0.41(#11), 0.39 to 0.44(#12), 0.40 to 0.45(#13), 0.44 to 0.49(#14), 0.54 to 0.59(#15), 0.56 to 0.61(#16), 0.58 to 0.63(#17), 0.72 to 0.77(#18), 0.74 to 0.79(#19), 0.78 to 0.83(#20), 0.82 to 0.87(#21), 0.84 to 0.89(# 1.01 to 0.89), 1.01 to 0.89(# 23), and 0.01 to 0.89(# 3); taking the schisandrin as a reference peak, and the relative peak areas of the 24 characteristic peaks are respectively as follows: 0.37 to 0.42(#1), 0.078 to 0.083(#2), 1.93 to 1.98(#3), 0.064 to 0.069(#4), 0.22 to 0.27(#5), 0.14 to 0.19(#6), 0.48 to 0.53(#7), 0.92 to 0.97(#8), 0.18 to 0.23(#9), 0.21 to 0.26(#10), 0.45 to 0.50(#11), 0.09 to 0.14(#12), 2.93 to 2.98(#13), 0.31 to 0.36(#14), 0.13 to 0.18), 0.08 to 0.13(#16), 0.26 to 0.31(#17), 0.26 to 0.31(#18), 0.09 to 0.14(#19), 0.08 to 0.13), 0.20 to 0.25), 0.20 to 0.21 (# 0.15) (# 0.05 to 0.05) (#15) (# 0.05) and (# 10).
B. In the HPLC fingerprint of the pulse-activating injection preparation, the schisandrin is taken as a reference peak, and the relative retention time of 26 characteristic peaks is respectively as follows: 0.043(#1), 0.056(#2), 0.066(#3), 0.080(#4), 0.092(#5), 0.120(#6), 0.186(#7), 0.252(#8), 0.290(#9), 0.303(#10), 0.321(#11), 0.340(#12), 0.408(#13), 0.422(#14), 0.465(#15), 0.520(#16), 0.582(#17), 0.596(#18), 0.744(#19), 0.813(# 20), 0.21 (#21), 0.834(#22), 0.863(#23), 0.934 24), 1.000(#25), 1.029(# 26); taking the schizandrol A as a reference peak, and the relative peak areas of the 26 characteristic peaks are respectively as follows: 0.251(#1), 0.270(#2), 0.769(#3), 3.203(#4), 0.989(#5), 1.073(#6), 13.945(#7), 0.331(#8), 0.287(#9), 1.231(#10), 0.328(#11), 0.200(#12), 0.315(#13), 3.659(#14), 0.332(#15), 0.227(#16), 0.200(#17), 0.445(#18), 0.272(#19), 0.132(#20), 0.196(#21), 0.112(#22), 0.080(#23), 0.247(#24), 1.000(#25), and 0.084(# 26).
(C) By comparing the relative retention time and the relative peak area of the characteristic peak of the schisandra chinensis medicinal material and the relative retention time and the relative peak area of the characteristic peak of the pulse-activating injection preparation, the corresponding characteristic peaks between the schisandra chinensis medicinal material and the pulse-activating injection preparation are obtained, and the characteristic peaks #3, #9, #13, #23, #24 in the schisandra chinensis medicinal material are found to correspond to the characteristic peaks #4, #8, #14, #25, #26 in the pulse-activating injection preparation, so that the correlation between the schisandra chinensis medicinal material and the pulse-activating injection preparation is evaluated.
In conclusion, the method for constructing the high performance liquid chromatography fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof establishes an analysis method of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof, is used for evaluating the correlation between the medicinal materials and the preparation, and realizes the quality control from the medicinal materials to the preparation; according to the application of the HPLC fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof, the HPLC fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof is established, the relative content of main components in the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof is accurately analyzed and determined, and the product quality can be effectively and reliably predicted according to the content, so that the quality of the medicinal material and the correlation between the medicinal material and the preparation can be comprehensively evaluated.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (5)
1. An application of HPLC fingerprint spectrum of fructus Schisandrae and SHENGMAI injection preparation is characterized by absorbing the absorptionInjecting the test solution of the schisandra chinensis medicinal material and the pulse activating injection preparation test solution into a liquid chromatograph for high performance liquid chromatography analysis to obtain an HPLC fingerprint of the schisandra chinensis medicinal material and an HPLC fingerprint of the pulse activating injection preparation, wherein the conditions of the liquid chromatography are as follows: waters symmetry shieldTMRP18A chromatographic column; the detection wavelength is 250-260 nm, and the flow rate of the mobile phase is 0.8-1.3 mL/min-1The column temperature is 26-40 ℃; the mobile phase A is acetonitrile, the mobile phase B is a phosphoric acid water solution with the volume percentage of 0.02% -0.04%, and the mobile phase A and the mobile phase B are subjected to gradient elution; by comparing and analyzing the HPLC fingerprint of the schisandra chinensis medicinal material and the HPLC fingerprint of the shengmai injection preparation with the characteristic peaks in the HPLC fingerprint of the schizandrol A reference solution, the relative contents of the main components in the schisandra chinensis medicinal material and the shengmai injection preparation are obtained;
the requirements for gradient elution are as follows, where the ratio between mobile phase a and mobile phase B is the volume ratio:
at 0min, mobile phase a: mobile phase B = 0: 100, respectively;
at 17min, mobile phase a: mobile phase B = 4: 96;
at 20min, mobile phase a: mobile phase B = 10: 90, respectively;
at 40min, mobile phase a: mobile phase B = 15: 85 parts by weight;
at 60min, mobile phase a: mobile phase B = 60: 40;
at 70min, mobile phase a: mobile phase B = 95: 5;
at 75min, mobile phase a: mobile phase B = 95: 5;
at 80min, mobile phase a: mobile phase B = 0: 100.
2. the application of the HPLC fingerprint construction method of schisandra chinensis medicinal material and the pulse-activating injection preparation thereof according to claim 1, wherein the method is characterized in that Waters symmetry shieldTMRP18The size of the column was 4.6mm × 250mm, 5.0 μm.
3. The application of the HPLC fingerprint construction method of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof according to claim 1, wherein the preparation method of the schisandra chinensis medicinal material test solution is as follows: weighing fructus Schisandrae, adding purified water, decocting, filtering, and collecting filtrate as fructus Schisandrae test solution; the pulse activating injection preparation test solution is prepared according to the pulse activating injection preparation process.
4. The application of the construction method of the HPLC fingerprint of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof according to claim 1, characterized in that the HPLC fingerprint of the schizandrol A reference solution is obtained by injecting the schizandrol A reference solution into a liquid chromatograph for high performance liquid chromatography analysis.
5. The application of the HPLC fingerprint construction method of the schisandra chinensis medicinal material and the pulse-activating injection preparation thereof according to claim 4, wherein the preparation method of the schizandrol A reference solution is as follows: weighing the schizandrol A, adding methanol and mixing to obtain a schizandrol A reference substance solution, wherein the content of the schizandrol A in the schizandrol A reference substance solution is 8-13 mu g/ml.
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