CN113740198B - Method for measuring yellow vaseline content in musk hemorrhoid ointment - Google Patents
Method for measuring yellow vaseline content in musk hemorrhoid ointment Download PDFInfo
- Publication number
- CN113740198B CN113740198B CN202110943835.0A CN202110943835A CN113740198B CN 113740198 B CN113740198 B CN 113740198B CN 202110943835 A CN202110943835 A CN 202110943835A CN 113740198 B CN113740198 B CN 113740198B
- Authority
- CN
- China
- Prior art keywords
- musk
- content
- yellow
- sample
- yellow vaseline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229940099259 vaseline Drugs 0.000 title claims abstract description 82
- 208000014617 hemorrhoid Diseases 0.000 title claims abstract description 58
- 241000402754 Erythranthe moschata Species 0.000 title claims abstract description 57
- 239000002674 ointment Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 44
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 241000555676 Malassezia Species 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000004264 Petrolatum Substances 0.000 claims description 18
- 229940066842 petrolatum Drugs 0.000 claims description 18
- 235000019271 petrolatum Nutrition 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 5
- 241000208140 Acer Species 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 47
- 239000000243 solution Substances 0.000 description 20
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 12
- 238000000605 extraction Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000012488 sample solution Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- 239000004166 Lanolin Substances 0.000 description 6
- 229940116229 borneol Drugs 0.000 description 6
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 6
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- 229940039717 lanolin Drugs 0.000 description 6
- 235000019388 lanolin Nutrition 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000013642 negative control Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013558 reference substance Substances 0.000 description 4
- 238000012795 verification Methods 0.000 description 4
- 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 3
- 230000005526 G1 to G0 transition Effects 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000012088 reference solution Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 244000153234 Hibiscus abelmoschus Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 229940105847 calamine Drugs 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 229960001760 dimethyl sulfoxide Drugs 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 229910052864 hemimorphite Inorganic materials 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 235000014692 zinc oxide Nutrition 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- CPYIZQLXMGRKSW-UHFFFAOYSA-N zinc;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+3].[Fe+3].[Zn+2] CPYIZQLXMGRKSW-UHFFFAOYSA-N 0.000 description 2
- 206010004542 Bezoar Diseases 0.000 description 1
- 239000003390 Chinese drug Substances 0.000 description 1
- 240000000783 Origanum majorana Species 0.000 description 1
- 235000006297 Origanum majorana Nutrition 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- -1 borax Chemical compound 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000003255 drug test Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000007430 reference method Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a method for measuring the yellow vaseline content in a musk hemorrhoids ointment of a malassezia, which comprises the steps of (1) taking a musk hemorrhoids ointment sample of the malassezia, adding ethanol, heating, stirring, dissolving, cooling, filtering, and discarding filtrate to obtain residues; (2) Washing the residue with chloroform for multiple times, mixing the residue and the washing liquid, performing ultrasonic treatment to dissolve yellow vaseline therein, cooling to room temperature, fixing the volume with chloroform, and filtering to obtain filtrate; (3) And (3) evaporating the filtrate in a bath, drying in a baking oven, cooling, weighing to obtain the weight of the yellow vaseline, and carrying out conversion by combining the weight of the sample of the musk haemorrhoids paste of the Makino so as to obtain the content of the yellow vaseline in the musk haemorrhoids paste of the Makino. The method is extremely simple, high in precision and accuracy, good in reliability and less in interference.
Description
Technical Field
The invention relates to content determination of traditional Chinese medicine components, in particular to a method for determining the content of yellow vaseline in a musk hemorrhoids ointment of Maxiong.
Background
The ointment, ma Ying Long musk hemorrhoid ointment, is a pure Chinese medicinal preparation prepared from artificial musk, artificial bezoar, pearl, calcined calamine powder, borax, borneol and amber, and is a national Chinese medicinal protection variety. Besides the main components, the ointment also contains auxiliary materials such as yellow vaseline, lanoline and the like, and in order to ensure the efficacy of the product, strict quality control is required to be carried out on all links from purchasing, checking, accepting and warehousing of the raw auxiliary materials, the whole production process to intermediate product control, checking and measuring of the finished product and the like in the whole preparation process of the finished ointment. At present, only yellow vaseline serving as an auxiliary material in the musk hemorrhoids ointment of the maple is detected, and the content of the yellow vaseline in the preparation is not controlled. Therefore, in order to better control the product quality, the drug standard of the Ma Ying Longshan hemorrhoid ointment which is received in one part of the Chinese pharmacopoeia is improved and researched according to the requirements of the analysis method verification guidelines of the drug quality standard of the Chinese pharmacopoeia 2020 edition. The new quality standard is added with the determination of the yellow vaseline content, a determination method of the yellow vaseline content in the preparation is established by adopting a weight method, and the content limit is set.
Because yellow vaseline is an auxiliary material in the prescription, no ready-made reference method is available for measuring the content of the yellow vaseline. Through patent inquiry, the 104502291B patent discloses a method for measuring the content of vaseline in civil double-base powder, which sequentially comprises the following steps: processing the sample into a sheet; the sample is fully rinsed by the circulating evaporation and condensation extractant to extract the sample; directly evaporating the extracting agent from the extracted extracting solution to obtain an extract; adding excess tetrahydrofuran to dissolve vaseline in the extract and transferring to a volumetric flask and metering with tetrahydrofuran; accurately transferring the solution into another volumetric flask, adding acetonitrile water solution to precipitate vaseline, shaking to constant volume, and measuring absorbance of the suspension; and calculating the content of the Vaseline by the measured absorbance and a standard curve. The method calculates the content of Vaseline by the measured absorbance and a standard curve. Because the gunpowder components are relatively simple, the yellow vaseline is relatively easy to separate, and the content of the yellow vaseline can be measured by an ultraviolet standard curve method. The musk hemorrhoids ointment of the malassezia is complex in components, and auxiliary materials similar to yellow vaseline in nature also exist in the auxiliary materials, so that the content of the yellow vaseline in the hemorrhoids ointment cannot be measured by the method.
On the other hand, yellow petrolatum is a semisolid mixture of various hydrocarbons obtained from petroleum, and the contents of the components in yellow petrolatum produced each time are not uniform due to its complex composition. Therefore, when the method is used for measuring the content of yellow vaseline in the musk hemorrhoids ointment of the Makino, the content cannot be detected simply by preparing a reference substance for content detection, and the conventional gas chromatography and liquid chromatography cannot detect the content. And for the Makino musk hemorrhoid ointment with complex traditional Chinese medicine components, other extraction methods are adopted, and other auxiliary materials are interfered. For this purpose, yellow vaseline must be effectively extracted for content measurement by utilizing different physical properties of each component in the product.
Disclosure of Invention
The invention aims to solve the technical problems and provide a method for measuring the yellow vaseline content in the musk hemorrhoids ointment with extremely simple method, high precision and accuracy, good reliability and little interference.
The invention discloses a method for measuring the content of yellow vaseline in a musk hemorrhoids ointment, which comprises the following steps:
(1) Taking a musk hemorrhoid ointment sample of the malassezia, adding ethanol, heating in water bath, stirring for dissolution, cooling, filtering, and discarding the filtrate to obtain residues;
(2) Washing the residue with chloroform for multiple times, mixing the residue and the washing liquid, performing ultrasonic treatment to dissolve yellow vaseline, cooling to room temperature, fixing volume with chloroform, and filtering to obtain filtrate;
(3) And (3) evaporating the filtrate in a water bath, drying in an oven, cooling, weighing to obtain the weight of the yellow vaseline, and carrying out conversion by combining the weight of the sample of the musk haemorrhoids paste of the Makino so as to obtain the content of the yellow vaseline in the musk haemorrhoids paste of the Makino.
In the step 1), the water bath heating temperature is 98 percent ～ Stirring for 5 minutes at 100 ℃; freezing in a refrigerator with a temperature of-5 ℃ for 30 minutes. The sampling amount of the sample of the musk hemorrhoids ointment with the maple is 4-6g.
In the step 2), the ultrasonic treatment conditions are as follows: power 200W, frequency 53kHz; ultrasound for 10 minutes.
In the step 2), the filtering method is filter paper filtering.
In the step 3), the water bath evaporating temperature is 98-100 ℃, the drying temperature is 105 ℃, the drying time is 2.5 hours, and the cooling time is 30 minutes.
Aiming at the problems in the background art, the method of weighing the yellow Vaseline after extracting the yellow Vaseline is considered to calculate the content of the yellow Vaseline in the Makino musk hemorrhoid ointment, and the method is simple, but because the Makino musk hemorrhoid ointment is a traditional Chinese medicine composition, the components are complex, and some components have similar properties with Huang Fanlin, such as lanolin and the like. In the extraction process, in order to ensure the precision and accuracy, the yellow vaseline is extracted as much as possible, and the purity of the yellow vaseline is ensured to be high without impurity interference, so that the accuracy requirement of the weighing method for measuring the content can be met. In this regard, the inventors have conducted intensive analyses on the components of the musk hemorrhoid ointment, by utilizing the property that yellow vaseline and other components in the musk hemorrhoid ointment have different solubilities in different solvents, ethanol is first used to mix with the musk hemorrhoid ointment and then heated to dissolve, at this time lanolin, dimethyl sulfoxide, borneol and artificial musk in the musk hemorrhoid ointment are then dissolved into an ethanol solution, while yellow vaseline is insoluble in hot ethanol and remains in the residue after cooling. The components of lanolin, dimethyl sulfoxide, borneol and artificial musk can be separated by adopting a cooling and filtering mode; furthermore, the inventor utilizes the characteristic that yellow vaseline is dissolved in chloroform, and other components such as borax, calcined calamine powder and the like are insoluble, and selects the yellow vaseline to wash physical filter residues for multiple times, and in order to improve the extraction rate, the residues and washing liquid are combined for ultrasonic treatment after multiple times of washing, and the ultrasonic power is preferably 200W and the frequency is 53kHz; ultrasonic time is 10 minutes, and too short ultrasonic time can lead to incomplete dissolution of yellow vaseline. Filtering to remove residue, evaporating filtrate, and drying in 105 deg.C oven to remove residual solvent and volatile substances such as Borneolum Syntheticum and dimethyl sulfoxide.
The determination method is extremely simple, the yellow vaseline with high purity can be obtained by only one-time extraction, the extraction rate is high, the impurity interference is less, the method has the advantages of good accuracy, high precision, low cost and good reliability, and the quantitative detection of the yellow vaseline can be satisfied, so that the quality of the musk hemorrhoids ointment with the Chinese moschus is effectively ensured.
Drawings
FIG. 1 is a blank solvent gas chromatogram.
FIG. 2 is a gas chromatogram of yellow Vaseline control solution.
FIG. 3 is a gas chromatogram of a sample solution of a musk hemorrhoids ointment of the Makino type.
FIG. 4 is a linear plot of different sample amounts versus yellow petrolatum content.
FIG. 5 is a gas chromatogram of a solution of a musk extract of musk hemorrhoids.
FIG. 6 is a gas chromatogram of a negative control sample solution.
Detailed Description
1. Determination of content determination method
1.1 determination of yellow Vaseline content in Makino musk hemorrhoid ointment by gas chromatography
1.1.1 preliminary establishment of extraction and analysis methods
Since yellow petrolatum is a semi-solid mixture of various hydrocarbons derived from petroleum, we diluted yellow petrolatum control with cyclohexane to a solution of about 5mg/ml and a sample of the musk hemorrhoids cream with cyclohexane to a solution of about 6 mg/ml. Analyzing yellow vaseline reference solution and Makino Moschus hemorrhoid ointment sample solution by gas chromatography under the following conditions:
a capillary column (column length of 30m, inner diameter of 0.32mm, film thickness of 1.0 μm) with 5% phenyl-95% methylpolysiloxane as stationary phase; the initial temperature is 35 ℃, the temperature is raised to 320 ℃ at the rate of 15 ℃ per minute, and the temperature is maintained for 40 minutes; the temperature of the sample inlet is 360 ℃; the detector temperature was 360℃under chromatographic conditions, the carrier gas was nitrogen, and the sample volume was 1. Mu.l.
Results: referring to FIGS. 1 to 3, yellow vaseline has 15 characteristic absorption peaks such as S4 to S18 at 15 minutes to 28 minutes. And (3) preliminarily determining 15 peaks such as S4-S18 and the like as main component peaks, and calculating the yellow Vaseline content in the Makinong musk hemorrhoid ointment by an external standard method by using the sum of the peak areas of the main components.
1.1.2 detection of sample content
Measured by gas chromatography.
Chromatographic conditions: a capillary column (column length of 30m, inner diameter of 0.32mm, film thickness of 1.0 μm) with 5% phenyl-95% methylpolysiloxane as stationary phase; the initial temperature is 35 ℃, the temperature is raised to 320 ℃ at the rate of 15 ℃ per minute, and the temperature is maintained for 40 minutes; the temperature of the sample inlet is 360 ℃; the detector temperature was 360 ℃ under chromatographic conditions and the carrier gas was nitrogen.
Correction factor measurement: taking appropriate amount of yellow Vaseline reference substance, precisely weighing, and diluting with cyclohexane to obtain 5mg/ml solution. 1ul of the extract was injected into a gas chromatograph, and a correction factor was calculated.
Assay: taking 0.3g of musk hemorrhoids ointment of the malassezia, precisely weighing, placing the ointment into a beaker, ultrasonically dissolving the ointment with 30ml of cyclohexane, pouring the ointment into a 100ml volumetric flask, washing the ointment with cyclohexane for 3 times, 20ml each time, combining the washing liquid into the volumetric flask, cooling the ointment to room temperature, fixing the volume to scales, and shaking the ointment evenly. Sucking 1ul, injecting into gas chromatograph, and measuring.
Test lot number: 20110011, 20110012, 20120011
The results of measuring the yellow petrolatum content of the three batches of samples according to the method described above are shown in Table 1:
TABLE 1
| Lot number | 20110011 | 20110012 | 20120011 |
| Content of | 95.5％ | 85.3％ | 107.5％ |
Results: the measurement result is greatly different from the theoretical value (about 77.99%), and the method cannot accurately measure the yellow vaseline content in the musk hemorrhoids ointment.
Analyzing the reason: firstly, the response value and the concentration of each component in yellow vaseline are not in a direct proportion relation, and the accuracy of a simple measuring method for calculating the content through area addition cannot meet the inspection requirement; second, the control used was a yellow petrolatum control from the chinese drug testing institute, which was used for identification purposes only, and the ingredients and specific contents were unknown. ( Remarks: yellow vaseline reference substances for content determination are not available in Chinese medicine verification institute. )
1.2 determination of yellow Vaseline content by gravimetric method
Inventive example 1: precisely weighing 5.0g of the product, adding 50ml of ethanol, heating in water bath at 98-100 ℃, stirring for 5 minutes, cooling in a refrigerator at-5 ℃ for 30 minutes, filtering with filter paper, and discarding the filtrate. Washing the residue with chloroform, repeatedly washing the residue on filter paper with chloroform, mixing the residue and the washing liquid in 50ml volumetric flask, ultrasonic treating (power 200W, frequency 53 kHz) for 10min to dissolve yellow vaseline completely, cooling to room temperature, and fixing volume to scale with chloroform. Filtering, taking 25ml of the subsequent filtrate into an evaporation dish with constant weight at 105 ℃, evaporating in water bath (98-100 ℃) to dryness, drying in an oven at 105 ℃ for 2.5 hours, taking out the filtrate into a dryer, cooling for 30 minutes, rapidly weighing, and calculating the content of yellow vaseline in the sample. The calculation formula is as follows: weigh weight x 2/sample weight x 100%.
1.2.1 extraction times comparative example 1:
extracting with hot ethanol twice: 2g (sample 1 and sample 2) and 4g (sample 3 and sample 4) of musk hemorrhoids ointment of the malassezia are respectively taken, precisely weighed, 50ml of ethanol is added, the mixture is heated and stirred in a water bath for 5 minutes, the mixture is cooled in a refrigerator at the temperature of minus 5 ℃ for 30 minutes, filter paper is used for filtration, the filtrate is removed, 50ml of ethanol is added to residues, and the steps are repeated, and the other steps are the same as in example 1.
The content percentages are shown in Table 2: (in theory, the yellow vaseline content of the sample was 77.99%)
TABLE 2
| Sample number | Sample 1 | Sample 2 | Sample 3 | Sample 4 |
| Content (%) | 64.4％ | 51.8％ | 72.0％ | 56.3％ |
Results: from the content results, the extraction is better than the extraction of two results, and the result with larger sampling amount is closer to the theoretical value.
1.2.2 sample size and drying time comparative example 1:
4g, 5g, 6g and 7g of musk hemorrhoids ointment of the malassezia are respectively taken, precisely weighed, 50ml of ethanol is added, the operation is the same as in example 1, the mixture is put into a baking oven at 105 ℃ for drying for 0.5 hour, 2.5 hours and 3.5 hours after being evaporated to dryness in a water bath, and the mixture is taken out to a dryer, cooled for 30 minutes and then quickly weighed.
The content percentages are shown in Table 3: (in theory, the yellow vaseline content of the sample was 77.99%)
TABLE 3 Table 3
Results: from the results of the content, the solid content was almost unchanged at a drying time of 2.5 hours and a drying time of 3.5 hours, and from the economical point of view, the drying time was 2.5 hours. The sampling amounts were 5g and 6g, the solid results were similar and all were close to the theoretical value (theoretical 77.99% of yellow vaseline in the sample).
Conclusion: the sampling amount is 4-6g, and the drying time is more than 2.5h. The content of yellow vaseline can be detected well.
1.2.3 extraction reagent comparative example 1:
respectively weighing 5.0g of each of four samples, precisely weighing, selecting chloroform and cyclohexane for comparison as extraction reagents (two samples in each group), adding 50ml of ethanol, heating and stirring in water bath for 5 minutes, cooling in a refrigerator at-5 ℃ for 30 minutes, filtering with filter paper, discarding filtrate, dissolving chloroform group residues with 30ml of chloroform, dissolving cyclohexane group residues with 30ml of cyclohexane with ultrasound, and carrying out ultrasonic conditions and subsequent treatment in the same way as in example 1.
The content percentages are shown in Table 4: (in theory, the yellow vaseline content of the sample was 77.99%)
TABLE 4 Table 4
Results: from the content results, the chloroform group had better repeatability and solid content values than the cyclohexane group.
1.2.4 filtration mode comparative example 1:
four samples were weighed 5.0g each, precisely, and the treatment was the same as in example 1. Adding chloroform to a certain volume to scale, respectively centrifuging each group of two samples for 10min (3000 rpm), and collecting 25ml supernatant; (2) filtering with filter paper; 25ml of the subsequent filtrate was taken. The solutions obtained by the two different filtering modes are placed in an evaporation dish with constant weight at 105 ℃, dried in an oven at 105 ℃ after being evaporated in water bath for 2.5 hours, taken out to a dryer, cooled for 30 minutes and quickly weighed.
The content percentages are shown in Table 5: (in theory, the yellow vaseline content of the sample was 77.99%)
TABLE 5
Results: from the content results, the content values of the filter paper filtration are better than those of the centrifugation group.
2. Verification of content determination method
2.1 specificity test
Test lot number: 190401
Negative control sample: the results of the extraction of lanolin negative samples, borneol negative samples and yellow Vaseline negative samples according to the method of example 1 of the present invention to obtain yellow Vaseline content are shown in Table 6:
TABLE 6
| Lot number | 190401 | Lanolin negative sample | Negative sample of borneol | Yellow Vaseline negative sample |
| Content of | 78.4％ | 80.8％ | 81.8％ | 0.8％ |
Results: in the special test, the detection results of the lanolin negative sample and the borneol negative sample are basically consistent with the theoretical values, and the yellow Vaseline negative sample has little residue, but is acceptable in a linear range.
2.2 accuracy test (recovery test)
6 parts of a musk hemorrhoid ointment (MHI in the United states of America, outlet) (batch No. 190401) with known content are precisely weighed by adopting a sample adding and recycling test, reference raw materials are precisely added respectively, a sample of yellow vaseline is extracted by operating the method of the embodiment 1 of the invention, and the recycling rate of the yellow vaseline in the sample is calculated, and the result is shown in Table 7.
TABLE 7
Results: the recovery rate of 6 parts of 100% concentration level standard sample solution is between 95 and 102%, and the average recovery rate is 97.93%; the RSD value is 1.06% and less than 1.5%, which indicates that the method is accurate.
2.3 precision test
The same batch of samples (batch No. 190401) was taken and the content of 6 parallel samples was determined according to the method of example 1 of the present invention. RSD values for yellow petrolatum content in 6 parallel samples were calculated and the results are shown in table 8.
TABLE 8
Results: the RSD of the sample content reproducibility was 0.63% and the reproducibility of the method was good.
2.4 linearity and Range
2.4.1 Linear
Precisely weighing 1g, 2g, 3g, 4g, 5g and 6g of control raw materials, operating according to the method of the embodiment 1 of the invention, and finally placing the control raw materials in 6 constant weight evaporation dishes and drying the control raw materials at 105 ℃ for 2.5 hours to obtain 6 control raw materials for linear experiments with different contents.
A linear regression equation was performed on the measured yellow petrolatum content and the sampled amount, and the results are shown in Table 9:
table 9 linear range test results
Results: referring to fig. 4, a linear regression equation of the sampled amount of yellow petrolatum versus the mass of yellow petrolatum: y= 1.0333x-0.2327, correlation coefficient r2=0.9999, n=6. The sampling amount of yellow vaseline is in the range of 1.0148 g-6.0131 g, and the linear relation is good.
2.4.2 Range
10 batches of musk hemorrhoids cream (Outlet USA) were prepared and tested for yellow petrolatum content according to the method of example 1 of the present invention, and the results are shown in Table 10:
table 10
According to the calculation of the preparation method, the yellow vaseline content in the product is 77.99%, the yellow vaseline content in the musk hemorrhoids ointment of the Makino is detected by different personnel for 10 batches of products according to the method, the yellow vaseline content is between 74.6 and 79.5%, and the operating errors among different laboratories are considered, so that the yellow vaseline content range in the musk hemorrhoids ointment of the Makino is specially designed to be 70.2 to 85.8%.
2.5 re-verification of the method by gas chromatography
Test lot number: 20120011
Negative control sample: male musk hemorrhoid ointment negative sample (yellow-free vaseline)
The extract solution of the musk hemorrhoids extract of the Majorana Hortensis: the test sample was extracted according to the method of example 1 of the present invention, 0.25g of the extract was precisely weighed, placed in a beaker, sonicated with 30ml of cyclohexane, poured into a 100ml volumetric flask, washed 3 times with 20ml of cyclohexane each time, and the washes were combined into the volumetric flask, cooled to room temperature, and then fixed to a scale, and shaken well.
Negative control sample solution: taking 0.1g of a musk hemorrhoids ointment negative sample (no yellow vaseline) of the malassezia, precisely weighing, placing the sample into a beaker, ultrasonically dissolving the sample with 30ml of cyclohexane, pouring the solution into a 100ml volumetric flask, washing the solution with cyclohexane for 3 times and 20ml each time, combining the washing solutions into the volumetric flask, cooling the solution to room temperature, fixing the volume to scales, and shaking the solution uniformly.
Control solution: taking appropriate amount of yellow Vaseline reference substance, precisely weighing, and diluting with cyclohexane to obtain 5mg/ml solution.
A capillary column (column length of 30m, inner diameter of 0.32mm, film thickness of 1.0 μm) with 5% phenyl-95% methylpolysiloxane as stationary phase; the initial temperature is 35 ℃, the temperature is raised to 320 ℃ at the rate of 15 ℃ per minute, and the temperature is maintained for 40 minutes; the temperature of the sample inlet is 360 ℃; the detector temperature was 360 ℃ under chromatographic conditions and the carrier gas was nitrogen.
Sucking 1 μl of extract solution of the hemorrhoids extract of Martensitic musk, yellow Vaseline negative sample solution and reference solution respectively, and injecting into gas chromatograph for detection.
Results: 15 characteristic absorption peaks such as chromatographic peaks S4-S18 in the solution chromatogram of the musk extract of Makino (figure 5) are consistent with those of the yellow vaseline reference solution chromatogram (figure 2); impurity peaks S1-S3 exist in the sample solution chromatogram (figure 3) of the musk hemorrhoids extract and the negative control sample solution chromatogram (figure 6), and the sample solution chromatogram (figure 5) of the musk hemorrhoids extract and the sample solution chromatogram (figure 2) of the yellow vaseline do not have impurity peaks S1-S3. The yellow vaseline extracted from the correction template has high purity and no impurity interference.
Claims (7)
1. A method for determining the yellow petrolatum content of a musk hemorrhoids ointment of a malassezia, comprising the steps of:
(1) Taking a musk hemorrhoid ointment sample of the malassezia, adding ethanol, heating in water bath, stirring for dissolution, cooling, filtering, and discarding the filtrate to obtain residues;
(2) Washing the residue with chloroform for multiple times, mixing the residue and the washing liquid, performing ultrasonic treatment to dissolve yellow vaseline therein, cooling to room temperature, fixing volume with chloroform, and filtering to obtain filtrate;
(3) And (3) evaporating the filtrate in a water bath, drying in an oven, cooling, weighing to obtain the weight of the yellow vaseline, and carrying out conversion by combining the weight of the sample of the musk haemorrhoids paste of the Makino so as to obtain the content of the yellow vaseline in the musk haemorrhoids paste of the Makino.
2. The method for determining the yellow petrolatum content of a musk hemorrhoid ointment according to claim 1, wherein the sample of the musk hemorrhoid ointment in step 1) is sampled in an amount of 4-6g.
3. The method for determining the yellow vaseline content in the musk hemorrhoid ointment of claim 1, wherein in step 1), the water bath heating temperature is 98-100 ℃, and the stirring time is 5 minutes; freezing in a refrigerator with a temperature of-5 ℃ for 30 minutes.
4. The method for determining the yellow petrolatum content of a musk hemorrhoid ointment according to claim 1, wherein in said step 1), the filtration is performed by using filter paper.
5. The method for determining the yellow petrolatum content of a mapuloone musk hemorrhoid ointment according to any one of claims 1-4, wherein in step 2), the ultrasonic conditions are controlled as follows: the power was 200W, the frequency was 53kHz, and the time was 10 minutes.
6. The method for determining the yellow petrolatum content of a maple musk hemorrhoid ointment according to any one of claims 1-4, wherein in step 2), the filtration is a filter paper filtration.
7. The method for determining the yellow petrolatum content of the musk hemorrhoid ointment according to any one of claims 1-4, wherein in the step 3), the temperature of the water bath evaporation to dryness is 98-100 ℃, the drying temperature is 105 ℃, the drying time is 2.5 hours, and the cooling time is 30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110943835.0A CN113740198B (en) | 2021-08-17 | 2021-08-17 | Method for measuring yellow vaseline content in musk hemorrhoid ointment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110943835.0A CN113740198B (en) | 2021-08-17 | 2021-08-17 | Method for measuring yellow vaseline content in musk hemorrhoid ointment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113740198A CN113740198A (en) | 2021-12-03 |
| CN113740198B true CN113740198B (en) | 2024-03-08 |
Family
ID=78731411
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110943835.0A Active CN113740198B (en) | 2021-08-17 | 2021-08-17 | Method for measuring yellow vaseline content in musk hemorrhoid ointment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113740198B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114652750B (en) * | 2022-03-08 | 2023-05-26 | 马应龙药业集团股份有限公司 | Application of traditional Chinese medicine composition in preparation of colorectal cancer prevention medicines |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033050A (en) * | 2011-01-13 | 2011-04-27 | 广东中烟工业有限责任公司 | Method for measuring pectin content in plant sample |
| CN103115841A (en) * | 2013-02-04 | 2013-05-22 | 合肥今越制药有限公司 | Quality control method for artificial calculus bovis raw material |
| CN105784914A (en) * | 2016-04-18 | 2016-07-20 | 山东明人福瑞达卫生材料有限公司 | Detection method for traditional Chinese medicine muskiness strong bone plasters |
| WO2017148418A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining component contents of chinese medicine composition |
| CN110596104A (en) * | 2019-09-18 | 2019-12-20 | 贵州医科大学 | Quality standard detection method for Hemerocallis citrina baroni medicinal material |
-
2021
- 2021-08-17 CN CN202110943835.0A patent/CN113740198B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033050A (en) * | 2011-01-13 | 2011-04-27 | 广东中烟工业有限责任公司 | Method for measuring pectin content in plant sample |
| CN103115841A (en) * | 2013-02-04 | 2013-05-22 | 合肥今越制药有限公司 | Quality control method for artificial calculus bovis raw material |
| WO2017148418A1 (en) * | 2016-03-03 | 2017-09-08 | 石家庄以岭药业股份有限公司 | Method for determining component contents of chinese medicine composition |
| CN105784914A (en) * | 2016-04-18 | 2016-07-20 | 山东明人福瑞达卫生材料有限公司 | Detection method for traditional Chinese medicine muskiness strong bone plasters |
| CN110596104A (en) * | 2019-09-18 | 2019-12-20 | 贵州医科大学 | Quality standard detection method for Hemerocallis citrina baroni medicinal material |
Non-Patent Citations (4)
| Title |
|---|
| 复方青黛软膏的制备与质量控制;黄开合;叶立红;田华;杨光义;王启斌;;医药导报(08);全文 * |
| 药用辅料凡士林的研究现状与应用;闫美玲等;海峡药学;第30卷(第9期);全文 * |
| 采用UV法测定黄凡士林中多环芳香烃的研究;海乐;刘雁鸣;;药物分析杂志(04);全文 * |
| 马应龙麝香痔疮膏质量标准的改进;孙德友, 李弘弢;药学实践杂志(01);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113740198A (en) | 2021-12-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105651924B (en) | The detection method of hormone in blood | |
| CN113702541B (en) | Poria cocos medicinal material characteristic spectrum construction method and poria cocos triterpene component detection method | |
| CN109324126B (en) | Method for simultaneously determining 9 chemical components in spina date seeds by using UPLC-MS/MS | |
| CN102520079B (en) | Method for rapidly measuring content of solanesol in tobaccos by using UPLC (Ultra Performance Liquid Chromatography) | |
| CN109406690B (en) | Method for detecting related substances in chloral hydrate | |
| CN109541117B (en) | Detection method of lung-moistening pharmaceutical composition | |
| CN113740198B (en) | Method for measuring yellow vaseline content in musk hemorrhoid ointment | |
| CN108072712B (en) | Quantitative analysis method for blood concentration of new compound WSJ-557 in SD rat plasma | |
| CN109765322B (en) | Method for constructing characteristic spectrum of schizonepeta and quality detection method | |
| CN105974016B (en) | It is a kind of while detect the method for Fosaprepitant and Aprepitant in blood plasma | |
| CN112014480A (en) | Method for detecting content of effective components in Jiangzhining granules by UPLC-MS/MS (ultra performance liquid chromatography-Mass Spectrometry/Mass Spectrometry) | |
| CN109541106A (en) | A kind of method that LC-MS measures frusemide concentration in blood plasma | |
| CN110031577B (en) | Quality detection method and identification application of traditional Chinese medicine or traditional Chinese medicine composition preparation | |
| CN104569265B (en) | Quality detection method of wine for relaxing muscles and tendons and treating rheumatism | |
| CN109917045B (en) | HPLC method for simultaneously measuring contents of 5 components in prepared rhizoma cibotii decoction pieces | |
| CN113109488A (en) | Method for extracting and detecting mometasone furoate in mometasone furoate gel | |
| CN106404685A (en) | Method for determination of total saponin content in health wine | |
| Li et al. | 1 H NMR determination of 1, 3-dicyclohexylurea, glutaric acid and triethylamine in medical four-arm poly (ethylene glycol)-N-hydroxysuccinimide-glutarate for better quality control | |
| CN110470751A (en) | Method that is a kind of while detecting 7 kinds of component contents in sharp capsule for treating gastropathy | |
| CN110297054A (en) | The detection method of Levetiracetam content in a kind of human serum | |
| CN107632075A (en) | Golden three kinds of component contents of bavin KANGGAN JIAONANG while assay method and its HPLC fingerprint map construction methods | |
| CN109828040B (en) | Construction method and detection method of UPLC (ultra Performance liquid chromatography) characteristic spectrum of eclipta medicinal material | |
| CN108627598A (en) | A method of measuring SC 59046 content | |
| CN113917010B (en) | Method for detecting effective components in eight-treasure pill capsule and application thereof | |
| CN106841462A (en) | The detection method of gallic acid in a kind of FRUCTUS TERMINALIAE IMMATURUS |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |