CN113740198A - Method for determining yellow vaseline content in Mayinglong musk hemorrhoid ointment - Google Patents
Method for determining yellow vaseline content in Mayinglong musk hemorrhoid ointment Download PDFInfo
- Publication number
- CN113740198A CN113740198A CN202110943835.0A CN202110943835A CN113740198A CN 113740198 A CN113740198 A CN 113740198A CN 202110943835 A CN202110943835 A CN 202110943835A CN 113740198 A CN113740198 A CN 113740198A
- Authority
- CN
- China
- Prior art keywords
- content
- yellow vaseline
- musk
- sample
- hemorrhoid ointment
- 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.)
- Granted
Links
- 229940099259 vaseline Drugs 0.000 title claims abstract description 89
- 208000014617 hemorrhoid Diseases 0.000 title claims abstract description 58
- 239000002674 ointment Substances 0.000 title claims abstract description 53
- 241000402754 Erythranthe moschata Species 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 45
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000005303 weighing Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 9
- 238000004821 distillation Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 52
- 239000000243 solution Substances 0.000 description 27
- 238000012360 testing method Methods 0.000 description 13
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 12
- 239000004264 Petrolatum Substances 0.000 description 11
- 229940066842 petrolatum Drugs 0.000 description 11
- 235000019271 petrolatum Nutrition 0.000 description 11
- 229960001701 chloroform Drugs 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 238000000605 extraction Methods 0.000 description 9
- 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
- 239000003814 drug Substances 0.000 description 7
- 239000013558 reference substance Substances 0.000 description 7
- 239000012488 sample solution 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
- 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
- 239000000463 material Substances 0.000 description 5
- 238000005259 measurement Methods 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
- 238000011084 recovery Methods 0.000 description 5
- -1 yellow vaseline Substances 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007787 solid Substances 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
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 230000005526 G1 to G0 transition Effects 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 235000005881 Calendula officinalis Nutrition 0.000 description 2
- 240000000785 Tagetes erecta 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
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application 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
- 238000004090 dissolution Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003721 gunpowder Substances 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
- 238000007689 inspection Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012088 reference solution Substances 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
- 238000012795 verification 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
- 244000153234 Hibiscus abelmoschus Species 0.000 description 1
- 229930184510 Mallotus Natural products 0.000 description 1
- 241001060384 Mallotus <angiosperm> Species 0.000 description 1
- 241000235395 Mucor Species 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 229960001760 dimethyl sulfoxide Drugs 0.000 description 1
- 238000003255 drug test Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 238000010812 external standard method 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
- 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
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000012419 revalidation Methods 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Images
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 Musk hemorrhoid ointment, which comprises (1) taking a Musk hemorrhoid ointment sample, adding ethanol, heating, stirring for dissolving, cooling, filtering, and removing filtrate to obtain residue; (2) washing the residue with chloroform for multiple times, combining the residue and washing liquid, performing ultrasonic treatment to dissolve yellow vaseline therein, cooling to room temperature, metering the volume of chloroform, and filtering to obtain filtrate; (3) drying the filtered liquid bath by distillation, placing the dried filtered liquid bath in an oven, cooling, weighing to obtain the weight of the yellow vaseline, and converting the weight of the Mayilong musk hemorrhoid ointment into the content of the yellow vaseline in the Mayilong musk hemorrhoid ointment by combining the weight of the Mayilong musk hemorrhoid ointment sample. 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 yellow vaseline content in a Mayinglong musk hemorrhoid ointment.
Background
The ointment Mayilong musk hemorrhoid ointment produced by Mayilong pharmaceutical industry group member company is a pure traditional Chinese medicine preparation refined by artificial musk, artificial bezoar, pearl, calcined calamine powder, borax, borneol and amber, and is a national traditional Chinese medicine protection variety. In addition to the main components, the ointment also contains auxiliary materials such as yellow vaseline, lanolin and the like, and in order to ensure the efficacy of the ointment, strict quality control must be performed on all links from raw material purchasing, acceptance and warehousing, the whole production process to intermediate product control, finished product inspection and measurement and the like in the whole preparation process of the finished ointment. At present, the auxiliary material yellow vaseline in the mayinglong musk hemorrhoid ointment is only detected on the raw materials, 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 Mayilong musk haemorrhoids ointment collected in the first part of the Chinese pharmacopoeia is improved and researched according to the requirements of the drug quality standard of the 'analysis method verification guiding principle' in the 'Chinese pharmacopoeia' 2020 edition. The new quality standard is added with the measurement of the yellow vaseline content, the method for measuring the yellow vaseline content in the preparation is established by adopting a gravimetric method, and the content limit is drawn up.
Because yellow vaseline is used as an auxiliary material in the prescription, the content of yellow vaseline cannot be determined by a ready-to-use reference method. Through patent inquiry, the patent 104502291B discloses a method for measuring the content of vaseline in civil double-base gunpowder, which sequentially comprises the following steps: processing the sample into a sheet shape; extracting the sample by circularly evaporating and condensing an extracting agent to fully rinse the sample; directly evaporating the extracting agent to obtain extract; adding excessive tetrahydrofuran to dissolve vaseline in the extract, transferring into a volumetric flask, and metering volume with tetrahydrofuran; accurately transferring the solution into another volumetric flask, adding acetonitrile aqueous solution to separate out vaseline, shaking to constant volume, and measuring absorbance of the suspension; and calculating the content of the vaseline by using the measured absorbance and a standard curve. The method calculates the content of vaseline by measuring the absorbance and a standard curve. Because the components of the gunpowder are relatively simple, the yellow vaseline is easy to separate, and the content of the yellow vaseline can be measured by an ultraviolet standard curve method. The mayinglong musk hemorrhoid ointment has complex components, and the auxiliary materials have the same properties with the yellow vaseline, so the content of the yellow vaseline cannot be determined by the recorded method.
On the other hand, yellow petrolatum is a semisolid mixture of various hydrocarbons obtained from petroleum, and the content of each component in yellow petrolatum obtained each time is not uniform due to its complex composition. Therefore, when the method is used for measuring the content of yellow vaseline in the Mayinglong musk hemorrhoid ointment, a reference substance cannot be simply prepared for content detection, and the content of the yellow vaseline cannot be detected by a conventional gas chromatography and a conventional liquid chromatography. For the Mayilong musk hemorrhoid ointment with complex traditional Chinese medicine components, other extraction methods are adopted, and the interference of other auxiliary materials also exists. Therefore, the yellow vaseline must be effectively extracted by utilizing different physical properties of each component in the product for content measurement.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for measuring the content of yellow vaseline in the marigold musk ointment for treating hemorrhoids, which has the advantages of simplicity, high precision and accuracy, good reliability and less interference.
The invention relates to a method for determining the content of yellow vaseline in a Mayinglong musk hemorrhoid ointment, which comprises the following steps:
(1) taking a Musk hemorrhoid ointment sample, adding ethanol, heating in water bath, stirring for dissolving, cooling, filtering, and removing filtrate to obtain residue;
(2) washing the residue with chloroform for multiple times, mixing the residue and washing liquid, performing ultrasonic treatment to dissolve yellow vaseline therein, cooling to room temperature, metering volume with chloroform, and filtering to obtain filtrate;
(3) drying the filtrate in a water bath to dryness, placing in an oven for drying, cooling, and weighing to obtain the weight of yellow vaseline, and converting into yellow vaseline in the Malayong musk hemorrhoid ointment by combining the weight of the Malayong hemorrhoid ointment sample.
In the step 1), the water bath heating temperature is 98 DEG～Stirring for 5 minutes at 100 ℃; the temperature was reduced to-5 ℃ for 30 minutes in a refrigerator. The sampling amount of the Mayilong musk hemorrhoid ointment sample is 4-6 g.
In the step 2), the ultrasonic treatment conditions are as follows: power 200W, frequency 53 kHz; sonicate for 10 minutes.
In the step 2), the filtering method is filter paper filtering.
In the step 3), the temperature of 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 min.
Aiming at the problems in the background art, the method for calculating the content of the yellow vaseline in the Mayilong musk hemorrhoid ointment by adopting the method of extracting the yellow vaseline and then weighing is considered, the method is simple, but the Mayilong musk hemorrhoid ointment is a traditional Chinese medicine composition, has complex components, and has similar properties with the yellow vaseline, such as lanolin and the like. In the extraction process, in order to ensure the precision and the 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 requirement on the accuracy of content measurement by a weighing method can be met. The inventor carries out deep analysis on the components of the Mayilong musk haemorrhoids paste, and utilizes the property that yellow vaseline and other components in the Mayilong musk haemorrhoids paste have different solubilities in different solvents, ethanol is firstly mixed with the Mayilong musk haemorrhoids paste, and then the mixture is heated and dissolved, wool fat, dimethyl sulfoxide, borneol and artificial musk in the Mayilong musk haemorrhoids paste are dissolved into ethanol solution, the yellow vaseline is insoluble in hot ethanol, and residues exist after cooling. The components of lanolin, dimethyl sulfoxide, borneol and artificial musk are separated by a cooling and filtering mode; furthermore, the inventor selects trichloromethane to wash physical filter residue for multiple times by utilizing the characteristic that yellow vaseline is dissolved in trichloromethane, and other components such as borax, calcined calamine powder and the like are insoluble, and also combines the residue and washing liquor to carry out ultrasonic treatment after multiple times of washing in order to improve the extraction rate, wherein the preferable ultrasonic power is 200W, and the frequency is 53 kHz; the ultrasonic treatment time is 10 minutes, and the yellow vaseline can not be completely dissolved due to too short ultrasonic treatment time. Filtering to remove residue after dissolving yellow vaseline, evaporating filtrate, and drying in oven at 105 deg.C 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 only by 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 can meet the requirement of quantitative detection of the yellow vaseline, so that the quality of the Moyonglong hemorrhoid ointment is effectively guaranteed.
Drawings
FIG. 1 is a blank solvent gas chromatogram.
Fig. 2 is a gas chromatogram of a yellow petrolatum control solution.
FIG. 3 is a gas chromatogram of a sample solution of Malilong musk hemorrhoid ointment.
FIG. 4 is a line graph of different sample sizes versus yellow petrolatum content.
FIG. 5 is a gas chromatogram of the solution of Malilong musk hemorrhoid extract.
FIG. 6 is a gas chromatogram of a negative control sample solution.
Detailed Description
1. Determination of assay method
1.1 gas chromatography for determining yellow vaseline content in Malycong musk ointment
1.1.1 preliminary establishment of extraction and analysis methods
Since yellow petrolatum is a semi-solid mixture of hydrocarbons obtained from petroleum, we diluted a yellow petrolatum control with cyclohexane to a solution of about 5mg/ml and a Mucor Moschwann hemorrhoid ointment sample with cyclohexane to a solution of about 6 mg/ml. Analyzing the yellow vaseline reference solution and the Mayilong musk hemorrhoid ointment sample solution by adopting a gas chromatography, wherein the chromatographic conditions are as follows:
a capillary column using 5% phenyl-95% methyl polysiloxane as a stationary phase (column length 30m, inner diameter 0.32mm, film thickness 1.0 μm); the initial temperature is 35 ℃, the temperature is increased to 320 ℃ at the rate of 15 ℃ per minute, and the temperature is maintained for 40 minutes; the temperature of a sample inlet is 360 ℃; the detector temperature was 360 ℃ chromatographic conditions, the carrier gas was nitrogen, and the sample volume was 1. mu.l.
As a result: referring to fig. 1-3, yellow vaseline has 15 characteristic absorption peaks such as S4-S18 at 15-28 minutes. Preliminarily determining 15 peaks such as S4-S18 and the like as main component peaks, and calculating the yellow vaseline content in the marigold hemorrhoid ointment by an external standard method according to the sum of the main component peak areas.
1.1.2 detection of sample content
Measured by gas chromatography.
Chromatographic conditions are as follows: a capillary column using 5% phenyl-95% methyl polysiloxane as a stationary phase (column length 30m, inner diameter 0.32mm, film thickness 1.0 μm); the initial temperature is 35 ℃, the temperature is increased to 320 ℃ at the rate of 15 ℃ per minute, and the temperature is maintained for 40 minutes; the temperature of a sample inlet is 360 ℃; the detector temperature was 360 ℃ chromatographic conditions and the carrier gas was nitrogen.
And (3) determination of a correction factor: taking a proper amount of yellow vaseline reference substance, precisely weighing, and diluting with cyclohexane to obtain a solution of 5 mg/ml. Sucking 1ul of the solution, injecting the solution into a gas chromatograph, and calculating a correction factor.
The determination method comprises the following steps: taking 0.3g of Musk hemorrhoid ointment, precisely weighing, placing in a beaker, ultrasonically dissolving with 30ml of cyclohexane, pouring into a 100ml volumetric flask, washing with cyclohexane for 3 times, 20ml each time, combining the washing liquids into the volumetric flask, cooling to room temperature, fixing the volume to the scale, and shaking up. Sucking 1ul of the solution, injecting the solution into a gas chromatograph, and measuring to obtain the product.
Test sample batch number: 20110011, 20110012, 20120011
The results of measuring the yellow petrolatum content in the three samples according to the above method are shown in table 1:
TABLE 1
| Batch number | 20110011 | 20110012 | 20120011 |
| Content (wt.) | 95.5％ | 85.3％ | 107.5％ |
As a result: the difference between the measurement result and the theoretical value (about 77.99%) is large, and the method cannot accurately measure the yellow vaseline content in the mayinglong musk hemorrhoid ointment.
The analysis reason is as follows: firstly, the response values and the concentrations of all components in the yellow vaseline are not in a direct proportion relationship, and the accuracy of a simple determination method for calculating the content by area addition cannot meet the inspection requirement; secondly, the used reference substance is purchased from yellow vaseline reference substance of China pharmaceutical examination research institute, which is only used for identification, and the components and specific content of the reference substance are unknown. (remark: yellow Vaseline reference substance for content determination is not available in Chinese institute for drug assay.)
1.2 gravimetric method determination of yellow Vaseline content
1.2.1 extraction times comparative example 1:
hot ethanol extraction was performed twice: respectively taking 2g (sample 1, sample 2) and 4g (sample 3, sample 4) of the Musk hemorrhoid ointment, precisely weighing, adding 50ml of ethanol, heating in water bath, stirring for 5 minutes, freezing in a refrigerator at-5 ℃ for 30min, filtering with filter paper, discarding the filtrate, adding 50ml of ethanol into the residue, and repeating the steps except for the step 1.
The content percentages are shown in table 2: (theoretical percentage of yellow vaseline in the sample is 77.99%)
TABLE 2
| | Sample | 1 | |
|
|
| Content (%) | 64.4％ | 51.8％ | 72.0％ | 56.3％ |
As a result: from the content results, the results obtained by extracting once are better than those obtained by extracting twice, and the results obtained by sampling a larger amount are closer to the theoretical value.
1.2.2 sample size and drying time comparative example 1:
respectively taking 4g, 5g, 6g and 7g of the Musk hemorrhoid ointment, precisely weighing, adding 50ml of ethanol, operating in the same example 1, drying by steaming in a water bath, respectively drying in a 105 ℃ oven for 0.5 hour, 2.5 hours and 3.5 hours, taking out into a dryer, cooling for 30 minutes, and rapidly weighing.
The content percentages are shown in table 3: (theoretical percentage of yellow vaseline in the sample is 77.99%)
TABLE 3
As a result: from the content results, when the drying time was 2.5 hours and the drying time was 3.5 hours, the solid content was almost unchanged, and from the economical point of view, the drying time was 2.5 hours. The solid results are similar when the sample amount is 5g and 6g, and the solid results are close to the theoretical value (the percentage of yellow vaseline in the sample is 77.99 percent theoretically).
And (4) conclusion: the sample is taken out of 4-6g, and the drying time is more than 2.5 h. The content of yellow vaseline can be well detected.
1.2.3 extraction reagents comparative example 1:
weighing four samples respectively 5.0g, precisely weighing, selecting chloroform and cyclohexane as extraction reagents (each two samples), adding 50ml ethanol, heating in water bath, stirring for 5 min, freezing in a refrigerator at-5 ℃ for 30min, filtering with filter paper, discarding filtrate, adding 30ml chloroform into chloroform group residue for ultrasonic dissolution, adding 30ml cyclohexane into cyclohexane group residue for ultrasonic dissolution, and performing ultrasonic conditions and subsequent treatment in the same way as in example 1.
The content percentages are shown in table 4: (theoretical percentage of yellow vaseline in the sample is 77.99%)
TABLE 4
As a result: from the content results, the chloroform group has better repeatability and solid content value than the cyclohexane group.
1.2.4 filtration mode comparative example 1:
four samples, each 5.0g, were weighed separately and precisely weighed, and the treatment method was the same as in example 1. Adding trichloromethane to a constant volume to a scale, respectively centrifuging two samples of each group for 10min (3000 r/min) by adopting the step (1), and taking 25ml of supernate; (2) filtering with filter paper; 25ml of filtrate was taken. Putting the solutions obtained by the two different filtering modes into an evaporating dish with constant weight at 105 ℃, drying the solution by evaporation in a water bath, then putting the solution into an oven with the temperature of 105 ℃ for drying for 2.5 hours, taking the solution out of the dryer, cooling the solution for 30 minutes, and then quickly weighing the solution.
The content percentages are shown in table 5: (theoretical percentage of yellow vaseline in the sample is 77.99%)
TABLE 5
As a result: from the content results, the content value of the filter paper filtration is better than that of the centrifugal group.
2. Verification of content determination method
2.1 specificity test
Test sample batch number: 190401
Negative control samples: the results of the contents of the yellow vaseline obtained by extracting the lanolin negative sample, the borneol negative sample and the yellow vaseline negative sample by the method of the embodiment 1 of the invention are shown in Table 6:
TABLE 6
| Batch number | 190401 | Lanolin negative sample | Borneol negative sample | Yellow Vaseline negative sample |
| Content (wt.) | 78.4％ | 80.8％ | 81.8％ | 0.8％ |
As a result: in a specificity test, the detection results of a lanolin negative sample and a borneol negative sample are basically consistent with a theoretical value, and a yellow vaseline negative sample has a small residue and is acceptable in a linear range.
2.2 accuracy test (recovery test)
By adopting a sample-adding recovery test, 6 parts of the Mayilong musk hemorrhoid ointment (export American MHI) (batch number: 190401) with known content are precisely weighed, the control raw materials are respectively and precisely added, a yellow vaseline sample is extracted according to the method of the invention embodiment 1, and the recovery rate of the yellow vaseline in the sample is calculated, and the result is shown in Table 7.
TABLE 7
As a result: the recovery rate of 6 parts of the solution of the standard test sample with the concentration level of 100 percent is between 95 and 102 percent, and the average recovery rate is 97.93 percent; the RSD value is 1.06 percent and is less than 1.5 percent, which indicates that the method is accurate.
2.3 precision test
The same batch of samples (batch No. 190401) was taken and the contents of 6 replicates were determined in accordance with the procedure of example 1 of the present invention. The RSD values for the yellow petrolatum content in the 6 replicates were calculated and the results are shown in table 8.
TABLE 8
As a result: the RSD of the content repeatability of the sample is 0.63 percent, and the repeatability of the method is good.
2.4 linearity and Range
2.4.1 Linearity
Precisely weighing 1g, 2g, 3g, 4g, 5g and 6g of the reference raw materials, operating according to the method of the embodiment 1 of the invention, and finally drying in 6 constant weight evaporation dishes at 105 ℃ for 2.5h to obtain 6 reference raw materials for linear tests with different contents.
The linear regression equation was performed with the measured yellow petrolatum content and the sample size, and the results are shown in table 9:
TABLE 9 Linear Range test results
As a result: referring to fig. 4, a linear regression equation of the sampled amount of yellow petrolatum with the mass of yellow petrolatum: y is 1.0333x-0.2327, correlation coefficient R2 is 0.9999, and n is 6. The result shows that the sampling amount of the 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 Malilong musk hemorrhoids ointment (exported in the United states) are taken, the yellow vaseline content is respectively measured according to the method of the invention in the embodiment 1, and the results are shown in a table 10:
watch 10
In the first part of the '2020 edition of Chinese pharmacopoeia', the content of yellow vaseline in the product is 77.99% calculated according to the preparation method, the content of yellow vaseline in the Mayilong musk haemorrhoids ointment detected by different persons according to the method for 10 batches of products is 74.6% -79.5%, and the content of yellow vaseline in the specially-prepared Mayilong musk haemorrhoids ointment is 70.2% -85.8% by considering the operation errors among different laboratories.
2.5 revalidation of the method by gas chromatography
Test sample batch number: 20120011
Negative control samples: mayinglong musk hemorrhoid ointment negative sample (non-yellow vaseline)
Mayinglong musk hemorrhoid extract solution: taking a sample to be tested, extracting according to the method of the embodiment 1 of the invention, taking 0.25g of extract, precisely weighing, placing in a beaker, ultrasonically dissolving with 30ml of cyclohexane, pouring into a 100ml volumetric flask, washing with cyclohexane for 3 times, 20ml each time, combining washing liquids into the volumetric flask, cooling to room temperature, fixing the volume to the scale, and shaking up.
Negative control sample solution: taking 0.1g of Mallotus hemorrhoid ointment negative sample (without yellow vaseline), precisely weighing, placing in a beaker, ultrasonically dissolving with 30ml of cyclohexane, pouring into a 100ml volumetric flask, washing with cyclohexane for 3 times, 20ml each time, combining the washing solutions into the volumetric flask, cooling to room temperature, fixing the volume to the scale, and shaking up.
Control solution: taking a proper amount of yellow vaseline reference substance, precisely weighing, and diluting with cyclohexane to obtain a solution of 5 mg/ml.
A capillary column using 5% phenyl-95% methyl polysiloxane as a stationary phase (column length 30m, inner diameter 0.32mm, film thickness 1.0 μm); the initial temperature is 35 ℃, the temperature is increased to 320 ℃ at the rate of 15 ℃ per minute, and the temperature is maintained for 40 minutes; the temperature of a sample inlet is 360 ℃; the detector temperature was 360 ℃ chromatographic conditions and the carrier gas was nitrogen.
Respectively sucking 1 μ l each of the Mayilong Moschus hemorrhoid extract solution, yellow Vaseline negative sample solution, and control solution, and injecting into gas chromatograph for detection.
As a result: 15 characteristic absorption peaks such as chromatographic peaks S4-S18 in the chromatogram (figure 5) of the hemorrhoid extract solution of the Mayilong musk are consistent with the chromatogram (figure 2) of the yellow vaseline reference solution; the chromatogram of the Mayilong musk haemorrhoids paste sample solution (figure 3) and the chromatogram of the negative control sample solution (figure 6) both have impurity peaks S1-S3, and the chromatogram of the Mayilong musk haemorrhoids paste extract solution (figure 5) and the chromatogram of the yellow vaseline control sample solution (figure 2) have no 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 measuring the content of yellow vaseline in a Mayinglong musk hemorrhoid ointment is characterized by comprising the following steps:
(1) taking a Musk hemorrhoid ointment sample, adding ethanol, heating in water bath, stirring for dissolving, cooling, filtering, and removing filtrate to obtain residue;
(2) washing the residue with chloroform for multiple times, combining the residue and washing liquid, performing ultrasonic treatment to dissolve yellow vaseline therein, cooling to room temperature, metering volume with chloroform, and filtering to obtain filtrate;
(3) drying the filtrate in a water bath to dryness, placing in an oven for drying, cooling, and weighing to obtain the weight of yellow vaseline, and converting into yellow vaseline in the Malayong musk hemorrhoid ointment by combining the weight of the Malayong hemorrhoid ointment sample.
2. The method for determining the yellow vaseline content in a mayinlong musk hemorrhoid ointment of claim 1, wherein in step 1), the sample size of a mayinlong musk hemorrhoid ointment sample is 4-6 g.
3. The method for determining the content of yellow vaseline in the mayinglong musk hemorrhoid ointment as claimed in claim 1, wherein in the step 1), the water bath heating temperature is 98-100 ℃, and the stirring time is 5 minutes; the temperature was reduced to-5 ℃ for 30 minutes in a refrigerator.
4. The method for determining the yellow vaseline content of a mayilong musk hemorrhoid ointment of claim 1, wherein in the step 1), the filtering is performed by using filter paper.
5. The method for determining the yellow vaseline content in a mayinglong musk hemorrhoid ointment according to any one of claims 1 to 4, wherein in the 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 vaseline content of a mayilong musk ointment for hemorrhoids of any one of claims 1 to 4, wherein in the step 2), the filtration is filter paper filtration.
7. The method for determining the content of yellow vaseline in a mayilong musk hemorrhoid ointment according to any one of claims 1 to 4, wherein in the step 3), the temperature for evaporating to dryness in a water bath is 98-100 ℃, the drying temperature is 105 ℃, the drying time at DEG C is 2.5 hours, and the cooling time is 30 min.
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 true CN113740198A (en) | 2021-12-03 |
| CN113740198B 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) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114652750A (en) * | 2022-03-08 | 2022-06-24 | 马应龙药业集团股份有限公司 | Application of traditional Chinese medicine composition in preparation of medicine for preventing colorectal cancer |
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 | A quality standard detection method of Shui Huang Hua 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 | A quality standard detection method of Shui Huang Hua medicinal material |
Non-Patent Citations (4)
| Title |
|---|
| 孙德友, 李弘?|: "马应龙麝香痔疮膏质量标准的改进", 药学实践杂志, no. 01 * |
| 海乐;刘雁鸣;: "采用UV法测定黄凡士林中多环芳香烃的研究", 药物分析杂志, no. 04 * |
| 闫美玲等: "药用辅料凡士林的研究现状与应用", 海峡药学, vol. 30, no. 9 * |
| 黄开合;叶立红;田华;杨光义;王启斌;: "复方青黛软膏的制备与质量控制", 医药导报, no. 08 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114652750A (en) * | 2022-03-08 | 2022-06-24 | 马应龙药业集团股份有限公司 | Application of traditional Chinese medicine composition in preparation of medicine for preventing colorectal cancer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113740198B (en) | 2024-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108072727B (en) | Method for simultaneously determining residual quantity of 23 organochlorine pesticides in pseudo-ginseng | |
| CN109633041B (en) | Determination of dihydrotestosterone in medicine by derivatization HPLC | |
| CN102520079B (en) | Method for rapidly measuring content of solanesol in tobaccos by using UPLC (Ultra Performance Liquid Chromatography) | |
| CN105651924B (en) | The detection method of hormone in blood | |
| CN113933445A (en) | A kind of Dendrobium standard decoction quality control method | |
| CN109406690B (en) | Method for detecting related substances in chloral hydrate | |
| CN108061774B (en) | Method for simultaneously determining residual quantity of 19 organochlorine pesticides in pseudo-ginseng | |
| CN108693265A (en) | The extraction and purifying of HERBA DENDROBII total alkaloid and content assaying method | |
| CN106483084A (en) | A kind of method of Total saponin in SPE colorimetric method for determining American Ginseng | |
| CN113740198A (en) | Method for determining yellow vaseline content in Mayinglong musk hemorrhoid ointment | |
| CN106645518A (en) | Method for determining residual quantity of chloramphenicol in propolis | |
| CN109856270A (en) | A method of with 7 index components in hplc simultaneous determination canopy powder granule | |
| CN104931519A (en) | Content detection method of salvianolic acid injection liquid | |
| CN115575546B (en) | Construction method of HPLC fingerprint of Wuziyanzong soft capsule and content determination method | |
| CN113759037B (en) | Characteristic spectrum of formula granules of semen lepidii and/or semen lepidii as well as construction method and identification method thereof | |
| CN111579684B (en) | Method for measuring content of total capsaicin in capsule wall material of capsule | |
| CN114646690B (en) | Detection method for chemical components in immature bitter orange, longstamen onion bulb and cassia twig decoction and fingerprint establishment method | |
| CN115032310A (en) | A kind of detection method of 6 kinds of dianthrones in Polygonum multiflorum | |
| CN114858935A (en) | HPLC (high Performance liquid chromatography) characteristic spectrum construction method and detection method of dampness-removing and pain-relieving fluid extract | |
| CN115266964A (en) | Method for detecting nitrosamine genotoxic impurities in losartan potassium | |
| CN115060840A (en) | HPLC quality control method for white flower paulownia leaf sesame oil preparation | |
| CN112946136A (en) | Method for determining content of mesylate in ozesamicin | |
| CN113759011A (en) | Method for establishing characteristic spectrum of starwort root and preparation thereof | |
| CN111650312A (en) | Quality detection method of wine for relaxing muscles and tendons and treating rheumatism | |
| CN111122761A (en) | Method for detecting sodium butyrate in feed by gas chromatograph |
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 |