CN112924594B - Method for measuring content of levo-muscone - Google Patents
Method for measuring content of levo-muscone Download PDFInfo
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- CN112924594B CN112924594B CN202110266403.0A CN202110266403A CN112924594B CN 112924594 B CN112924594 B CN 112924594B CN 202110266403 A CN202110266403 A CN 202110266403A CN 112924594 B CN112924594 B CN 112924594B
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- 238000000034 method Methods 0.000 title claims abstract description 19
- ALHUZKCOMYUFRB-OAHLLOKOSA-N Muscone Chemical compound C[C@@H]1CCCCCCCCCCCCC(=O)C1 ALHUZKCOMYUFRB-OAHLLOKOSA-N 0.000 claims abstract description 30
- ALHUZKCOMYUFRB-UHFFFAOYSA-N muskone Natural products CC1CCCCCCCCCCCCC(=O)C1 ALHUZKCOMYUFRB-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000741 silica gel Substances 0.000 claims abstract description 6
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 6
- 239000000945 filler Substances 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 13
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 12
- 239000005695 Ammonium acetate Substances 0.000 claims description 12
- 241000402754 Erythranthe moschata Species 0.000 claims description 12
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 12
- 229940043376 ammonium acetate Drugs 0.000 claims description 12
- 235000019257 ammonium acetate Nutrition 0.000 claims description 12
- 239000013558 reference substance Substances 0.000 claims description 11
- FACFHHMQICTXFZ-UHFFFAOYSA-N 2-(2-phenylimidazo[1,2-a]pyridin-3-yl)ethanamine Chemical compound N1=C2C=CC=CN2C(CCN)=C1C1=CC=CC=C1 FACFHHMQICTXFZ-UHFFFAOYSA-N 0.000 claims description 9
- 229940067137 musk ketone Drugs 0.000 claims description 9
- 239000012085 test solution Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 239000012088 reference solution Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000003814 drug Substances 0.000 description 5
- JHGWQSGWUPCKNT-UHFFFAOYSA-N 2-tert-butyl-4-methyl-1,3,5-trinitrobenzene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C(C(C)(C)C)=C1[N+]([O-])=O JHGWQSGWUPCKNT-UHFFFAOYSA-N 0.000 description 4
- 241001416180 Moschidae Species 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 241000972155 Moschus Species 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XDFUNZJKZIEFPV-UHFFFAOYSA-N 1-(2,3,8,8-tetramethyl-1,3,4,4a,5,6,7,8a-octahydronaphthalen-2-yl)ethanol Chemical compound C1C(C)C(C(O)C)(C)CC2C1CCCC2(C)C XDFUNZJKZIEFPV-UHFFFAOYSA-N 0.000 description 1
- 241000972159 Moschus chrysogaster Species 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- G01N30/16—Injection
-
- 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
-
- 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
-
- 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
- G01N30/60—Construction of the column
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for measuring the content of levo-muscone, wherein a chromatographic column takes silica gel coated with amylose-tri [ (S) -alpha-methyl phenyl carbamate ] on the surface as a filling agent. Measuring the content of levorotatory muscone by high performance liquid chromatography at 283 nm. The results show that the levorotatory muscone has good linear relation in the range of 0.5mg/ml to 10mg/ml, and the regression equation is that y is 0.5x +2.038, and r is 0.9997. The method has the advantages of high sensitivity, simplicity, convenience and rapidness and strong applicability, and can be used as an effective method for detecting the levorotatory muscone.
Description
Technical Field
The application belongs to the field of muscone content determination, and particularly relates to a levorotatory muscone content determination method.
Background
Levo muscone, CAS: 10403-00-6, English name l-Muscone, is optically isomeric with dextro Muscone, and has a molecular formula of C16H30O, molecular weight 238.412. Is the main effective component of musk.
The Moschus is dry secretion of mature male sachet of forest musk deer moschus berezovski Flerov, horse musk deer M.sifanicus Przewalski or original musk deer M.moscheffersus Linnaeus. Has effects of inducing resuscitation, refreshing mind, promoting blood circulation, dredging channels, relieving swelling and pain, and can be used for treating common diseases, frequently encountered diseases and difficult and complicated diseases. At present, more than 400 Chinese patent medicines are received in the Chinese pharmacopoeia, and musk is taken as a key raw material. The musk deer hunted for a long time is fragrant, and musk deer resources are seriously damaged, so that a plurality of Chinese patent medicines are difficult to form, and therefore, the artificial musk is organized by the joint attack and customs cooperation group which is led by the pharmaceutical research institute of Chinese medical academy of sciences after entrusted by the Ministry of health and Chinese medicinal materials, and is successfully developed to replace the musk after the research of nearly 20 years. At present, the replacement rate of the artificial musk is over 99 percent, thereby not only meeting the drug use requirements of people, but also avoiding the hunting of national first-level protection animal musk deer and making great contribution to the ecological environment of China.
The muscone in the artificial musk is racemic body, contains two components of levorotatory muscone and dextrorotatory muscone, and through research, the fragrance of levorotatory muscone is full and strong, and is main active component, and the muscone in the natural musk is also levorotatory muscone, so in order to ensure that the levorotatory muscone content in the artificial musk is consistent with the natural musk, it is especially important to establish a detection method of levorotatory muscone in the medicine.
Besides having important application in the aspect of medicines, the levorotatory muscone is also a representative variety of fragrant macrocyclic musk, has sweet aroma, can be well blended with various spices, has extremely low aroma threshold value (0.001ppm-0.01ppm), has lasting aroma and is an extremely effective aroma fixative. The musk is added into the high-grade painting and calligraphy, so that the painting and calligraphy have elegant and fragrant smell and are anticorrosive and mothproof. Therefore, the detection method of the levo-muscone is particularly important.
Disclosure of Invention
In order to solve the problems, the application provides a method for measuring the content of levorotatory muscone, which sequentially comprises the following steps:
s1: preparing a musk test solution;
weighing a sample containing muscone, placing the sample into a 100ml conical flask, adding 50ml of 90% acetonitrile water solution, carrying out ultrasonic treatment for 20min, taking out, filtering, placing 25ml of subsequent filtrate into a 50ml volumetric flask, adding 90% acetonitrile water solution, and fixing the volume to the scale to obtain the musk ketone;
s2: a reference solution of levo-muscone;
weighing levo-muscone reference substance, placing into a 100ml volumetric flask, adding 90% acetonitrile water solution for dissolving, and fixing the volume to scale to obtain the levo-muscone reference substance;
s3: the content of levo-muscone is determined by high performance liquid chromatography.
Preferably, the column is packed with silica gel coated with amylose-tris [ (S) - α -methylphenyl carbamate ] on the surface.
Preferably, the mixed solvent of ammonium acetate solution and acetonitrile is used as a mobile phase, the pH value is adjusted to 4.0 by using acetic acid, and the content of the levorotatory muscone is measured by using a high performance liquid chromatography at 283 nm.
Preferably, the concentration of the ammonium acetate solution is 0.05-0.5 mol/L.
Preferably, the mass ratio of the ammonium acetate solution to the acetonitrile is 20: (80-100).
Preferably, the flow rate of the mobile phase is 0.5 ml/min.
Preferably, the loading amount is 5-10 μ l.
This application can bring following beneficial effect:
1. the detection method disclosed by the invention is used for detecting the levorotatory muscone, and the sample is simple to prepare, stable and good in repeatability;
2. the detection method has the advantages of high sensitivity, simplicity, convenience and quickness and strong applicability.
Detailed Description
Example 1: a method for measuring the content of levo-muscone comprises the following steps:
s1: preparing a musk test solution;
weighing 3g of a sample containing musk ketone, placing the sample into a 100ml conical flask, adding 50ml of 90% acetonitrile water solution, carrying out ultrasonic treatment for 20min, taking out the sample, filtering, placing 25ml of subsequent filtrate into a 50ml volumetric flask, adding 90% acetonitrile water solution, and fixing the volume to the scale to obtain the musk ketone;
s2: a reference solution of levo-muscone;
weighing 0.3g of levo-muscone reference substance, precisely weighing, placing into a 100ml volumetric flask, adding 90% acetonitrile aqueous solution for dissolving, and fixing the volume to scale to obtain the levo-muscone reference substance;
s3: determining the content of levo-muscone by high performance liquid chromatography, wherein the chromatographic conditions are as follows: the chromatographic column takes silica gel coated with amylose-tri [ (S) -alpha-methylphenyl carbamate ] on the surface as a filler, takes a mixed solvent of 0.05mol/L ammonium acetate solution and acetonitrile as a mobile phase, the flow rate is 0.5ml/min, and the loading amount is 10 mu L, wherein the mass ratio of the ammonium acetate solution to the acetonitrile is 20: 80, adjusting pH to 4.0 with acetic acid, and measuring l-muscone content by high performance liquid chromatography at 283 nm.
Example 2: a method for measuring the content of levo-muscone comprises the following steps:
s1: preparing a musk test solution;
weighing 4g of a sample containing muscone, placing the sample into a 100ml conical flask, adding 50ml of 90% acetonitrile water solution, carrying out ultrasonic treatment for 20min, taking out the sample, filtering, placing 25ml of subsequent filtrate into a 50ml volumetric flask, adding 90% acetonitrile water solution, and fixing the volume to the scale to obtain the musk ketone;
s2: a reference solution of levo-muscone;
weighing 0.4g of levo-muscone reference substance, precisely weighing, placing into a 100ml volumetric flask, adding 90% acetonitrile aqueous solution for dissolving, and fixing the volume to scale to obtain the levo-muscone reference substance;
s3: determining the content of levo-muscone by high performance liquid chromatography, wherein the chromatographic conditions are as follows: the chromatographic column takes silica gel coated with amylose-tri [ (S) -alpha-methylphenyl carbamate ] on the surface as a filler, takes a mixed solvent of 0.5mol/L ammonium acetate solution and acetonitrile as a mobile phase, the flow rate is 0.5ml/min, and the loading amount is 5 mu L, wherein the mass ratio of the ammonium acetate solution to the acetonitrile is 20: 95, adjusting pH to 4.0 with acetic acid, and measuring the content of levorotatory muscone by high performance liquid chromatography at 283 nm.
Example 3: a method for measuring the content of levo-muscone comprises the following steps:
s1: preparing a musk test solution;
weighing 5g of a sample containing muscone, placing the sample into a 100ml conical flask, adding 50ml of 90% acetonitrile water solution, carrying out ultrasonic treatment for 20min, taking out the sample, filtering, placing 25ml of subsequent filtrate into a 50ml volumetric flask, adding 90% acetonitrile water solution, and fixing the volume to the scale to obtain the musk ketone;
s2: a reference solution of levo-muscone;
weighing 0.4g of levo-muscone reference substance, precisely weighing, placing into a 100ml volumetric flask, adding 90% acetonitrile aqueous solution for dissolving, and fixing the volume to scale to obtain the levo-muscone reference substance;
s3: determining the content of levo-muscone by high performance liquid chromatography, wherein the chromatographic conditions are as follows: the chromatographic column takes silica gel coated with amylose-tri [ (S) -alpha-methylphenyl carbamate ] on the surface as a filler, takes a mixed solvent of 0.1mol/L ammonium acetate solution and acetonitrile as a mobile phase, the flow rate is 0.5ml/min, and the loading amount is 5 mu L, wherein the mass ratio of the ammonium acetate solution to the acetonitrile is 20: 100, adjusting pH to 4.0 with acetic acid, and measuring the content of levorotatory muscone by high performance liquid chromatography at 283 nm.
Experiments were carried out as described in examples 1-3 above, chromatograms were recorded, and the degree of separation of the chromatographic peaks and the number of theoretical plates were calculated, showing that the retention times of the levorotatory musk ketone component in the levorotatory musk ketone reference substance and the test substance were identical, the degree of separation was > 1.5 and the number of theoretical plates was > 3000.
The test is carried out on the control solution of 0.5mg/ml, 2mg/ml, 5mg/ml, 7mg/ml and 10mg/ml respectively, the peak area is plotted as the abscissa and the concentration is plotted as the ordinate, the result shows that the peak area and the concentration of the levorotatory muscone control show good linear relation, the levorotatory muscone has good linear relation in the range of 0.5mg/ml-10mg/ml, the regression equation is that y is 0.5x +2.038, and r is 0.9997.
Next, the precision and specificity of the method of the present invention were tested,
according to the chromatographic conditions of the example 1, 6 parts of the control solution prepared in the example 1 is adopted for measurement, a chromatogram is recorded, and the RSD value is calculated to be less than 2 percent, the experimental result is 0.7 percent and meets the requirement.
The control solution and the test solution were measured separately according to example 1, and the retention time and the degree of separation were recorded, showing that the levorotatory musk ketone chromatographic peak and other chromatographic peaks had a degree of separation of > 1.5 and no other impurity peaks were present.
The results show that the method is high in sensitivity, simple, convenient and quick, strong in applicability and can be used as an effective method for detecting the levorotatory muscone.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (4)
1. A method for measuring the content of levo-muscone is characterized by comprising the following steps:
s1: preparing a musk test solution;
weighing a sample containing muscone, placing the sample into a 100ml conical flask, adding 50ml of 90% acetonitrile water solution, carrying out ultrasonic treatment for 20min, taking out, filtering, placing 25ml of subsequent filtrate into a 50ml volumetric flask, adding 90% acetonitrile water solution, and fixing the volume to the scale to obtain the musk ketone;
s2: a reference solution of levo-muscone;
weighing levo-muscone reference substance, placing into a 100ml volumetric flask, adding 90% acetonitrile water solution for dissolving, and fixing the volume to scale to obtain the levo-muscone reference substance;
s3: measuring the content of levo muscone by high performance liquid chromatography;
in the step S3, the content of the L-muscone is measured by adopting a high performance liquid chromatography, the mobile phase is a mixed solvent of an ammonium acetate solution and acetonitrile, the pH value is adjusted to 4.0 by using acetic acid, and the content of the L-muscone is measured by utilizing the high performance liquid chromatography under 283 nm; the chromatographic column takes silica gel coated with amylose-tri [ (S) -alpha-methyl phenyl carbamate ] on the surface as a filling agent,
the volume ratio of the ammonium acetate solution to the acetonitrile is 20: (80-100).
2. The method for measuring the content of the levo-muscone according to claim 1, wherein: the concentration of the ammonium acetate solution is 0.05-0.5 mol/L.
3. The method for measuring the content of the levo-muscone according to claim 1, wherein: the flow rate of the mobile phase was 0.5 ml/min.
4. The method for measuring the content of the levo-muscone according to claim 1, wherein: the loading amount is 5-10 μ l.
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