CN108918718B - Detection method of hyoscyamine and scopolamine - Google Patents
Detection method of hyoscyamine and scopolamine Download PDFInfo
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- CN108918718B CN108918718B CN201810833435.2A CN201810833435A CN108918718B CN 108918718 B CN108918718 B CN 108918718B CN 201810833435 A CN201810833435 A CN 201810833435A CN 108918718 B CN108918718 B CN 108918718B
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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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid 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
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention relates to the technical field of chromatographic analysis, in particular to a detection method of hyoscyamine and scopolamine. The detection method adopts HPLC chromatographic analysis, and the chromatographic conditions are as follows: a chromatographic column: c18A chromatographic column; mobile phase A: acetonitrile; mobile phase B: the mixed solution of phosphoric acid and triethylamine, wherein the mass concentration of the phosphoric acid is 0.09-0.11%, and the volume concentration of the triethylamine is 0.015-0.025%; the gradient elution order was: 0-35 min: mobile phase A6%; 35-40 min: 6 to 30 percent of mobile phase A; 40-50 min: 30-6% of mobile phase A; flow rate of mobile phase: 0.9-1.1 mL/min; detection wavelength: 210 nm; column temperature of the chromatographic column: 34-36 ℃. According to the detection method provided by the invention, the peak of scopolamine and hyoscyamine has appropriate peak-producing time and good separation degree from the impurity peak.
Description
Technical Field
The invention relates to the technical field of chromatographic analysis, in particular to a detection method of hyoscyamine and scopolamine.
Background
Hyoscyamine, also known as henbane alkaloid, is one of belladonna alkaloids isolated from henbane and flos Daturae. Hyoscyamine has analgesic and spasmolytic effects, and can be used for treating sciatica, epilepsy, and seasickness.
Scopolamine has stronger toxicity than anthrax, can be fatal by taking a little excessive amount, is a tropane alkaloid, and exists in solanaceae plants. Scopolamine is an alkaloid with the strongest pharmacological action in belladonna, can be used for blocking parasympathetic nerve, can also be used as a central nervous system inhibitor, is generally a hydrobromide thereof clinically, can be used for anesthesia, analgesia, cough relief and asthma relief, is effective to motion sickness, and can also be used for controlling stiffness and tremor of Parkinson's disease.
Based on the toxicity of hyoscyamine and scopolamine, the content determination of hyoscyamine and scopolamine in the formulated preparation is very important, and the two components are difficult to detect respectively by using an HPLC method at present. In addition, the ingredients of the formulated preparation are complex, and the contents of hyoscyamine and scopolamine are low, so that the formulated preparation is difficult to extract from the formulated preparation, and the detection of the contents also forms a technical obstacle.
Disclosure of Invention
The invention provides a detection method of hyoscyamine and scopolamine, aiming at the problem that the hyoscyamine and scopolamine in the existing formula preparation are difficult to separate.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a detection method of hyoscyamine and scopolamine adopts HPLC chromatographic analysis, and the chromatographic conditions are as follows:
a chromatographic column: c18A chromatographic column;
mobile phase A: acetonitrile;
mobile phase B: the mixed solution of phosphoric acid and triethylamine, wherein the mass concentration of the phosphoric acid is 0.09-0.11%, and the volume concentration of the triethylamine is 0.015-0.025%;
the gradient elution order was:
0-35 min: mobile phase A6%;
35-40 min: 6 to 30 percent of mobile phase A;
40-50 min: 30-6% of mobile phase A;
flow rate of mobile phase: 0.9-1.1 mL/min;
detection wavelength: 210 nm;
column temperature of the chromatographic column: 34-36 ℃.
Compared with the prior art, the detection method of the hyoscyamine and the scopolamine provided by the invention adopts gradient elution, so that the hyoscyamine and the scopolamine in the test solution are well separated, the analysis period is shortened, the separation capacity is improved, the peak type is improved, and the sensitivity is increased.
Specifically, preferably, the method for preparing the sample solution for HPLC analysis from the formulated product at least comprises the following steps:
step a, sampling the prepared preparation, adding 75% ethanol by volume concentration, performing ultrasonic extraction, centrifuging, and evaporating supernatant to dryness to obtain a first residue;
b, dissolving the first residue in an ammonia solution, adding trichloromethane for ultrasonic extraction, extracting and separating an extracting solution to obtain a trichloromethane solution, and evaporating the trichloromethane solution to dryness to obtain a second residue;
c, adding methanol with the volume concentration of 50% into the second residue, and carrying out ultrasonic extraction to obtain an extracting solution, namely an extract containing hyoscyamine and scopolamine;
and d, transferring the supernatant of the extracting solution, and filtering by using a 0.45-micrometer filter membrane to obtain a test solution.
Preferably, when the formulation is a solid formulation, a sample is taken after milling; when the formulation is a liquid formulation, a sample is taken after evaporation to dryness.
Preferably, the sampling mass of the formula preparation in step a is 0.8-1.2 g.
Preferably, the ultrasonic extraction in the step a is carried out for 2 to 3 times, and the extraction time is 25 to 35min each time.
Preferably, the adding amount of the ethanol in the step a is 30-40 times of the sampling mass.
Preferably, the mass concentration of the ammonia solution in the step b is 2.0-2.5%, and 7-9mL of the concentrated ammonia solution is added with water to 100 mL.
Preferably, the mass of the ammonia solution in the step b is 17-22 times of the sampling mass.
Preferably, the chloroform in the step b is extracted by ultrasonic for 4 to 6 times, and the extraction time is 50 to 70s each time.
Preferably, the trichloromethane is added in an amount of 20 to 25 times the mass of the sample.
Preferably, the amount of methanol added in step c is 3-6 times of the sampling mass.
Preferably, the ultrasonic extraction in the step c is carried out for 4 to 6 times, and the extraction time is 50 to 70s each time.
The method for extracting the hyoscyamine and the scopolamine from the formulated preparation to prepare the test solution provides guarantee for accurately detecting the content of the hyoscyamine and the scopolamine in the formulated preparation.
Preferably, the HPLC chromatography uses a control solution prepared by the method comprising: dissolving scopolamine hydrobromide and atropine sulfate reference substances in 40-55% methanol to obtain standard stock solution, and diluting the standard stock solution to obtain reference substance solution, wherein 1mL of the reference substance solution contains 0.02g of scopolamine hydrobromide and 0.02g of atropine sulfate.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a liquid chromatogram of 50% methanol by volume provided by an embodiment of the present invention;
FIG. 2 is a liquid chromatogram of a control solution provided by an embodiment of the invention;
FIG. 3 is a liquid chromatogram of a test solution provided in an embodiment of the present invention;
FIG. 4 is a liquid chromatogram of a negative control solution provided by an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following examples are provided to better illustrate the embodiments of the present invention.
Example 1
The embodiment of the invention provides a detection method of hyoscyamine and scopolamine, and a prescription preparation adopts a stomach pain relieving tablet, wherein the stomach pain relieving tablet comprises the following components: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of liquorice dry extract, 25g of henbane extract, 155g of gentian powder and 4mL of fennel oil, wherein the henbane extract contains hyoscyamine and scopolamine.
The preparation method of the test solution of the Weitongning tablet comprises the following steps:
step a, grinding the solid preparation, sampling 1.0g, adding 34 times of 75% ethanol by volume, ultrasonically extracting for 3 times (30 min each time), centrifuging, combining supernate, and evaporating to dryness to obtain a first residue;
b, dissolving the first residue in 2.16% ammonia solution with the mass concentration 20 times of the sampling mass, adding trichloromethane with the mass 22 times of the sampling mass, carrying out ultrasonic extraction for 5 times for 60s each time, extracting and separating the extracting solution to obtain trichloromethane solution, combining the trichloromethane solution, and evaporating to dryness to obtain a second residue;
c, adding methanol with the volume concentration of 50% which is 4.4 times of the sampling mass into the second residue, carrying out ultrasonic extraction for 5 times, 60s each time, and combining the extracting solutions, wherein the extracting solution is an extract containing hyoscyamine and scopolamine;
and d, transferring the supernatant of the extracting solution into a 5mL volumetric flask, fixing the volume by adopting 50% methanol, shaking up, and filtering by using a 0.45 mu m filter membrane to obtain a test solution containing hyoscyamine and scopolamine.
Wherein the ammonia solution is prepared by adding 8mL of concentrated ammonia solution to 100mL of water.
The preparation method of the control solution of the stomach ache tablet comprises the following steps: dissolving scopolamine hydrobromide and atropine sulfate reference substances in 50% methanol to obtain standard stock solution, diluting the standard stock solution, and filtering with 0.45 μm filter membrane to obtain reference substance solution, wherein 1mL of the reference substance solution contains 0.02g of scopolamine hydrobromide and 0.02g of atropine sulfate.
The preparation method of the negative control solution of the stomach ache tablet comprises the following steps: according to the prescription proportion of the stomach pain relieving tablet: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of herba saponariae dry extract, 155g of gentian powder and 4mL of fennel oil, and the components are uniformly mixed, 1.0g of the mixture is taken, and the same preparation method is adopted as the sample solution of the Weitongning tablet, so that a negative sample solution which does not contain hyoscyamine and scopolamine is obtained.
Carrying out HPLC (high performance liquid chromatography) chromatographic analysis on methanol with the volume concentration of 50%, a test solution of a stomach pain relieving tablet, a reference solution of the stomach pain relieving tablet and a negative reference solution of the stomach pain relieving tablet, wherein the chromatographic conditions are as follows:
a chromatographic column: c18A chromatographic column;
mobile phase A: acetonitrile;
mobile phase B: the mixed solution of phosphoric acid and triethylamine, wherein the mass concentration of the phosphoric acid is 0.1 percent, and the volume concentration of the triethylamine is 0.02 percent;
the gradient elution order was:
0-35 min: mobile phase A6%;
35-40 min: 6 to 30 percent of mobile phase A;
40-50 min: 30-6% of mobile phase A;
flow rate of mobile phase: 1.0 mL/min;
detection wavelength: 210 nm;
column temperature of the chromatographic column: 35 ℃ is carried out.
Liquid chromatogram of 50% methanol, control solution of WEITONGNING tablet, test solution of WEITONGNING tablet, and negative control solution of WEITONGNING tablet are shown in FIG. 1, FIG. 2, FIG. 3, and FIG. 4, respectively.
The chromatogram of 50% by volume of methanol is shown in FIG. 1, in which the peak designated as 3, i.e., the peak of methanol, is shown.
The chromatogram of the control solution of the Weitongning tablet provided by the invention is shown in fig. 2, and as can be seen from fig. 2, the peak emergence time of scopolamine hydrobromide and atropine sulfate is appropriate, and the separation degree from the hetero peak is good, wherein, the peak 1 is the peak of scopolamine hydrobromide, and the peak 2 is the peak of atropine sulfate.
The chromatogram of the test solution of the gastralgia treating tablet provided by the invention is shown in fig. 3, and it is obvious from fig. 3 that the peak emergence time of scopolamine and hyoscyamine is appropriate, and the separation degree of the scopolamine and the hyoscyamine from the impurity peak is good, wherein the peak 1 is the peak of scopolamine, and the peak 2 is the peak of hyoscyamine.
The chromatogram of the negative control solution of the Weitongning tablet provided by the invention is shown in fig. 4, and as can be seen from fig. 4, except for the peak of methanol with the volume concentration of 50%, the other peaks are all mixed peaks, the peaks of scopolamine and hyoscyamine are not seen, and the separation degree of the mixed peaks is good.
Example 2
The embodiment of the invention provides a detection method of hyoscyamine and scopolamine, and a prescription preparation adopts a stomach pain relieving tablet, wherein the stomach pain relieving tablet comprises the following components: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of liquorice dry extract, 25g of henbane extract, 155g of gentian powder and 4mL of fennel oil, wherein the henbane extract contains hyoscyamine and scopolamine.
The preparation method of the test solution of the Weitongning tablet comprises the following steps:
step a, grinding the Weitongning tablets, sampling 1.2g, adding 40 times of ethanol with volume concentration of 70% by mass, ultrasonically extracting for 2 times, 35min each time, centrifuging, combining supernate, and evaporating to dryness to obtain first residues;
b, dissolving the first residue in 2.0% ammonia solution with the mass concentration being 22 times of the sampling mass, adding trichloromethane with the mass being 20 times of the sampling mass, carrying out ultrasonic extraction for 6 times, 50s each time, extracting and separating the extracting solution to obtain trichloromethane solution, combining the trichloromethane solution, and evaporating to dryness to obtain a second residue;
c, adding methanol with the volume concentration of 45 percent which is 3 times of the sampling mass into the second residue, carrying out ultrasonic extraction for 4 times, 50s each time, and combining the extracting solutions, wherein the extracting solution is the extract containing the hyoscyamine and the scopolamine;
and d, transferring the supernatant of the extracting solution into a 5mL volumetric flask, fixing the volume by adopting 50% methanol, shaking up, and filtering by using a 0.45 mu m filter membrane to obtain a test solution containing hyoscyamine and scopolamine.
Wherein the ammonia solution is 7.5mL of concentrated ammonia solution and is obtained by adding water to 100 mL.
The preparation methods of the control solution of the Weitongning tablet and the negative control solution of the Weitongning tablet are as described in example 1, and are not repeated.
Carrying out HPLC (high performance liquid chromatography) chromatographic analysis on methanol with the volume concentration of 50%, a test solution of a stomach pain relieving tablet, a reference solution of the stomach pain relieving tablet and a negative reference solution of the stomach pain relieving tablet, wherein the chromatographic conditions are as follows:
a chromatographic column: c18A chromatographic column;
mobile phase A: acetonitrile;
mobile phase B: the mixed solution of phosphoric acid and triethylamine, wherein the mass concentration of the phosphoric acid is 0.11 percent, and the volume concentration of the triethylamine is 0.025 percent;
the gradient elution order was:
0-35 min: mobile phase A6%;
35-40 min: 6 to 30 percent of mobile phase A;
40-50 min: 30-6% of mobile phase A;
flow rate of mobile phase: 1.1 mL/min;
detection wavelength: 210 nm;
column temperature of the chromatographic column: at 36 ℃.
The HPLC detection results of hyoscyamine and scopolamine in the formulated preparation provided in this example are the same as those in example 1, and are not repeated.
Example 3
The embodiment of the invention provides a detection method of hyoscyamine and scopolamine, and a prescription preparation adopts a stomach pain relieving tablet, wherein the stomach pain relieving tablet comprises the following components: 300g of dandelion extract, 300g of aluminum hydroxide, 210g of liquorice dry extract, 25g of henbane extract, 155g of gentian powder and 4mL of fennel oil, wherein the henbane extract contains hyoscyamine and scopolamine.
The preparation method of the test solution of the Weitongning tablet comprises the following steps:
step a, grinding the Weitongning tablets, sampling 0.8g, adding 30 times of ethanol with volume concentration of 80% by mass, ultrasonically extracting for 3 times, each time for 25min, centrifuging, combining supernate, and evaporating to dryness to obtain first residues;
b, dissolving the first residue in an ammonia solution with the mass concentration of 2.5% and the mass of 17 times that of the sample, adding trichloromethane with the mass of 25 times that of the sample, performing ultrasonic extraction for 4 times, each time for 70s, extracting and separating the extracting solution to obtain a trichloromethane solution, combining the trichloromethane solutions, and evaporating to dryness to obtain a second residue;
c, adding methanol with the volume concentration of 55% which is 6 times of the sampling mass into the second residue, carrying out ultrasonic extraction for 6 times, each time for 70s, and combining the extracting solutions, wherein the extracting solution is the extract containing hyoscyamine and scopolamine;
and d, transferring the supernatant of the extracting solution into a 5mL volumetric flask, fixing the volume by adopting 50% methanol, shaking up, and filtering by using a 0.45 mu m filter membrane to obtain a test solution containing hyoscyamine and scopolamine.
Wherein the ammonia solution is prepared by adding water to 100mL of concentrated ammonia solution 9 mL.
The preparation methods of the control solution of the Weitongning tablet and the negative control solution of the Weitongning tablet are as described in example 1, and are not repeated.
Carrying out HPLC (high performance liquid chromatography) chromatographic analysis on methanol with the volume concentration of 50%, a test solution of a stomach pain relieving tablet, a reference solution of the stomach pain relieving tablet and a negative reference solution of the stomach pain relieving tablet, wherein the chromatographic conditions are as follows:
a chromatographic column: c18A chromatographic column;
mobile phase A: acetonitrile;
mobile phase B: a mixed solution of phosphoric acid and triethylamine, wherein the mass concentration of the phosphoric acid is 0.09%, and the volume concentration of the triethylamine is 0.015%;
the gradient elution order was:
0-35 min: mobile phase A6%;
35-40 min: 6 to 30 percent of mobile phase A;
40-50 min: 30-6% of mobile phase A;
flow rate of mobile phase: 0.9 mL/min;
detection wavelength: 210 nm;
column temperature of the chromatographic column: at 34 ℃.
The HPLC detection results of hyoscyamine and scopolamine in the formulated preparation provided in this example are the same as those in example 1, and are not repeated.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A detection method of hyoscyamine and scopolamine in a tablet for treating stomachache is characterized in that: the detection method adopts HPLC chromatographic analysis, and the chromatographic conditions are as follows:
a chromatographic column: c18A chromatographic column;
mobile phase A: acetonitrile;
mobile phase B: the mixed solution of phosphoric acid and triethylamine, wherein the mass concentration of the phosphoric acid is 0.09-0.11%, and the volume concentration of the triethylamine is 0.015-0.025%;
the gradient elution order was:
0-35 min: mobile phase A6%;
35-40 min: 6% -30% of a mobile phase A;
40-50 min: 30% -6% of a mobile phase A;
flow rate of mobile phase: 0.9-1.1 mL/min;
detection wavelength: 210 nm;
column temperature of the chromatographic column: 34-36 ℃;
wherein the preparation method for preparing the sample solution for HPLC chromatographic analysis from the formulated preparation at least comprises the following steps:
step a, sampling the prepared preparation, adding 75% ethanol by volume concentration, performing ultrasonic extraction, centrifuging, and evaporating supernatant to dryness to obtain a first residue;
b, dissolving the first residue in an ammonia solution, adding trichloromethane for ultrasonic extraction, extracting and separating an extracting solution to obtain a trichloromethane solution, and evaporating the trichloromethane solution to dryness to obtain a second residue;
c, adding methanol with the volume concentration of 50% into the second residue, and carrying out ultrasonic extraction to obtain an extracting solution, namely an extract containing hyoscyamine and scopolamine;
and d, transferring the supernatant of the extracting solution, and filtering by using a 0.45-micrometer filter membrane to obtain a test solution.
2. The method for detecting hyoscyamine and scopolamine in a gastralgia tablet as claimed in claim 1, wherein: when the formulation is a solid formulation, a sample is taken after milling.
3. The method for detecting hyoscyamine and scopolamine in a gastralgia tablet as set forth in any one of claims 1 to 2, wherein: the sampling mass of the prescription preparation in the step a is 0.8-1.2 g; and/or
In the step a, ultrasonic extraction is carried out for 2-3 times, and the extraction time is 25-35min each time; and/or
The adding amount of the ethanol in the step a is 30-40 times of the sampling mass.
4. The method for detecting hyoscyamine and scopolamine in a gastralgia tablet as set forth in any one of claims 1 to 2, wherein: the mass concentration of the ammonia solution in the step b is 2.0-2.5%; and/or
The mass of the ammonia solution in the step b is 17-22 times of the sampling mass.
5. The method for detecting hyoscyamine and scopolamine in a gastralgia tablet as set forth in any one of claims 1 to 2, wherein: b, ultrasonically extracting the trichloromethane for 4-6 times, wherein the extraction time is 50-70s each time; and/or
The adding amount of the trichloromethane is 20-25 times of the sampling mass.
6. The method for detecting hyoscyamine and scopolamine in a gastralgia tablet as set forth in any one of claims 1 to 2, wherein: the adding amount of the methanol in the step c is 3-6 times of the sampling mass; and/or
And c, ultrasonic extraction is carried out for 4-6 times in the step c, and the extraction time is 50-70s each time.
7. The method for detecting hyoscyamine and scopolamine in a gastralgia tablet as claimed in claim 1, wherein: the method for preparing the reference substance solution for HPLC chromatographic analysis comprises the following steps: dissolving scopolamine hydrobromide and atropine sulfate reference substances in 40-55% methanol to obtain standard stock solution, and diluting the standard stock solution to obtain reference substance solution, wherein 1mL of the reference substance solution contains 0.02g of scopolamine hydrobromide and 0.02g of atropine sulfate.
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