CN115561353A - Method for measuring amount of ethanol in ergot maleate tablets - Google Patents
Method for measuring amount of ethanol in ergot maleate tablets Download PDFInfo
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- CN115561353A CN115561353A CN202211169602.0A CN202211169602A CN115561353A CN 115561353 A CN115561353 A CN 115561353A CN 202211169602 A CN202211169602 A CN 202211169602A CN 115561353 A CN115561353 A CN 115561353A
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 30
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 title claims abstract description 12
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000012085 test solution Substances 0.000 claims abstract description 11
- 239000012490 blank solution Substances 0.000 claims abstract description 8
- 239000012088 reference solution Substances 0.000 claims abstract description 7
- 238000010812 external standard method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 210000004907 gland Anatomy 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000011067 equilibration Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229940079593 drug Drugs 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 3
- 238000007689 inspection Methods 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000013558 reference substance Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- YREISLCRUMOYAY-BKQYHRSVSA-N (6ar)-n-(1-hydroxypropan-2-yl)-7-methyl-6,6a,8,9-tetrahydro-4h-indolo[4,3-fg]quinoline-9-carboxamide;(z)-but-2-enedioic acid Chemical compound OC(=O)\C=C/C(O)=O.C1=CC(C=2[C@H](N(C)CC(C=2)C(=O)NC(CO)C)C2)=C3C2=CNC3=C1 YREISLCRUMOYAY-BKQYHRSVSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NOFOWWRHEPHDCY-DAUURJMHSA-N Methylergonovine Maleate Chemical compound OC(=O)\C=C/C(O)=O.C1=CC(C=2[C@H](N(C)C[C@@H](C=2)C(=O)N[C@H](CO)CC)C2)=C3C2=CNC3=C1 NOFOWWRHEPHDCY-DAUURJMHSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 208000018525 Postpartum Hemorrhage Diseases 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000003255 drug test Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000005550 wet granulation Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to the field of drug analysis and detection, and provides a method for determining the amount of ethanol in ergot maleate tablets. The invention comprises the following steps: and respectively adding the blank solution, the reference solution and the test solution into a gas chromatograph, recording the chromatogram, and calculating the content of the residual ethanol in the ergot maleate tablet by peak area according to an external standard method. The method is rapid, efficient and low-toxic, has important significance for guiding enterprises to adjust process parameters and guaranteeing the medication safety of people, has short analysis time and low inspection cost, does not use more toxic and harmful reagents, and accords with the green industrialized development trend of the pharmaceutical industry in China.
Description
Technical Field
The invention belongs to the field of drug analysis and detection, and particularly relates to a method for determining the amount of ethanol in ergot maleate tablets.
Background
The ergometrine maleate is a first choice drug for treating postpartum hemorrhage internationally, the variety has no self-researched product on the market at home, in the process for preparing the ergometrine maleate tablet, ethanol is a tabletting step, a wetting agent is adopted for wet granulation, and in the subsequent drying step, the ethanol is theoretically completely removed, so if residual ethanol exceeding the national standard limit exists in the ergometrine maleate tablet, the indication process parameter is unreasonable to set, and further adjustment and improvement are needed, but no method for measuring the ethanol amount in the ergometrine maleate tablet exists at present.
Disclosure of Invention
The invention aims to solve the problems and provides a method for determining the amount of ethanol in ergot maleate tablets, which comprises the following steps:
respectively adding the blank solution, the reference solution and the test solution into a gas chromatograph, recording a chromatogram, and calculating the content of ethanol in the ergot maleate tablet by peak area according to an external standard method;
the chromatographic conditions are as follows:
a chromatographic column: agilent DB-624 (0.53 mm. Times.30m, 3 μm);
temperature programming: the initial column temperature was 40 ℃ for 5 minutes, at a rate of 10 ℃ per minute to 120 ℃ for 1 minute, and at a rate of 30 ℃ per minute to 240 ℃ for 2 minutes.
Sample inlet temperature: 250 ℃;
temperature of the detector: 280 ℃;
carrier gas: high purity nitrogen, flow rate: 3.0ml/min;
headspace bottle equilibrium temperature: 80 ℃, equilibration time: for 30 minutes.
Preferably, the blank solution is ultrapure water.
Preferably, the preparation of the control solution: accurately weighing 50mg of ethanol reference substance, placing in a 100ml measuring flask, diluting with water to scale, shaking, accurately weighing 2ml, placing in a top empty flask, and sealing with a gland.
Preferably, the preparation of the test solution is characterized by: 20 tablets of the product are taken and ground into fine powder, 0.2g of the fine powder is precisely weighed and placed in a 20ml headspace bottle, 2ml of water is accurately added, a gland is sealed, and the mixture is gently shaken for 10 minutes.
Compared with the prior art, the invention has the following beneficial effects:
the method adopts a gas chromatography-headspace sampling method, and measures the content of residual ethanol in the methylergometrine maleate tablet according to an external standard method and by calculating the peak area. The method is rapid, efficient and low-toxic, has important significance for guaranteeing the medication safety of people, has short analysis time and low inspection cost, does not use more toxic and harmful reagents in the method, and accords with the green industrialization development trend of the pharmaceutical industry in China.
Drawings
FIG. 1 is a typical map of system applicability;
FIG. 2 is a blank solution chromatogram;
FIG. 3 is a chromatogram of a control solution;
FIG. 4 is a chromatogram of a solution of a test sample (lot number: 200926);
FIG. 5 is a chromatogram of a solution of a sample (lot number 201002);
FIG. 6 is a chromatogram of a solution of a sample (lot number 201104).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
1. Instrument and reagent
The instrument comprises the following steps: agilent 7890B gas chromatograph;
a hydrogen Flame Ionization Detector (FID);
pure water hydrogen generator (resistivity 18.2 Ω);
SGK-2LB Low noise air Pump (Beijing Oriental essence park science, inc.);
an Open LBACDS Chem Station Edition workstation;
german mettler XS205 electron analytical balance.
Reagent: ultrapure water is self-made in laboratories.
Comparison products: ethanol, source: chinese food & drug assay research institute, lot number: 130106 to 202105, and the content is as follows: 100.0 percent
And (3) testing the sample: the methylergometrine maleate tablets are prepared by laboratories,
batch number: 200926, 201024, 201122.
2. Method of producing a composite material
2.1 chromatographic conditions
A chromatographic column: agilent DB-624 (0.53 mm. Times.30m, 3 μm);
temperature programming: the initial column temperature was 40 ℃ for 5 minutes, at a rate of 10 ℃ per minute to 120 ℃ for 1 minute, and at a rate of 30 ℃ per minute to 240 ℃ for 2 minutes.
Sample inlet temperature: 250 ℃;
detector temperature: 280 ℃;
carrier gas: high purity nitrogen, flow rate: 3.0ml/min;
headspace bottle equilibrium temperature: 80 ℃, equilibration time: for 30 minutes.
2.2 preparation of the solution
Preparing a blank solution: ultrapure water;
preparing a reference substance solution: accurately weighing 50mg of ethanol reference substance, placing in a 100ml measuring flask, diluting with water to scale, shaking, accurately weighing 2ml, placing in a top empty flask, and sealing with a gland.
Preparing a test solution: 20 tablets of the product are taken and ground into fine powder, 0.2g of the fine powder is precisely weighed and placed in a 20ml headspace bottle, 2ml of water is accurately added, a gland is sealed, and the mixture is gently shaken for 10 minutes.
Preparation of system applicability solution: and (3) sampling a control solution in a headspace manner, wherein the separation degree between a main peak and an adjacent impurity peak is more than 1.5.
3. Methodology validation
3.1 specificity experiments
The system applicability solution, the blank solution, the reference solution and the test solution are respectively injected into a gas chromatograph, and chromatograms are recorded, wherein the results are shown in figures 1 to 6.
The result shows that under the chromatographic condition, the solvent does not interfere with the sample measurement, and the ethanol peak and the front and rear impurity peaks can achieve baseline separation.
3.2 limit of quantitation and detection
Precisely measuring a reference substance solution, diluting step by step, injecting the reference substance solution into a gas chromatograph, and recording a chromatogram until the signal-to-noise ratio S/N is about 10, namely the quantitative limit;
and precisely measuring a reference substance solution, diluting the reference substance solution step by step, injecting the diluted reference substance solution into a gas chromatograph, and recording a chromatogram until the signal-to-noise ratio S/N is about 3, namely the detection limit.
Under the chromatographic conditions, the ethanol quantitative limit concentration is as follows: 15 μ g/ml, detection limit concentration: 5. Mu.g/ml.
3.3 linearity and Range
Accurately weighing 0.5011g of ethanol reference substance into a 100ml measuring flask, adding water to dilute to scale, shaking, accurately weighing 0.1ml, 1ml, 5ml, 10ml, 20ml and 30ml as reference substance stock solution, dividing into 100ml measuring flasks, adding water to dilute to scale, shaking to obtain standard solutions (1), (2), (3), (4) and (5) with concentrations of 5 μ g/ml, 50 μ g/ml, 0.25mg/ml, 0.5mg/ml and 1.0mg/ml respectively. And (5) carrying out sample injection measurement according to the chromatographic conditions, and recording the peak area. The corresponding concentration (C) was subjected to linear regression with peak area (a) and linear equation a =2590C-1.489, correlation coefficient r =0.9998. The results show that: the concentration of the ethanol is in the concentration range of 5 mu g/ml to 1.0mg/ml, and the concentration and the peak area have good linear relation.
3.4 accuracy
1 batch of the test sample (batch number: 201104) is taken, 0.2g of the test sample is precisely weighed, 9 parts of the test sample are parallelly weighed, the test sample is placed in a top empty bottle, 2ml of each of the standard solutions (3), (4) and (5) is respectively added, the test sample is sealed and slightly shaken for 10 minutes, the test sample is measured according to the method, a chromatogram is recorded, and the calculation is carried out according to an external standard method. The average recovery was 99.7% and the RSD was 1.2%, as shown in Table 1.
3.5 precision
3.5.1 repeatability
Taking 6 parts of reference solution, continuously injecting sample, and making the relative standard deviation of ethanol peak area be 0.55%
3.5.2 intermediate precision
1 batch of the test sample is taken. Batch number: 200926, preparing 6 parts of test solution according to the above method, injecting the test solution into a gas chromatograph, and determining that the average content of ethanol is 0.26% and the RSD is 0.7%;
3.6 stability
Taking the test solution and the reference solution, standing at room temperature, injecting into a gas chromatograph for 0h, 2h, 4h, 6h and 8h respectively, recording the peak area of ethanol, wherein RSD is 1.8% and 0.6% respectively, and the stability of the test solution and the reference solution is good within 8 hours in a solution state.
4. Sample assay
Taking 3 batches of samples prepared by a laboratory, and carrying out batch number: 200926, 201024, 201122, determined by the proposed injection method, the results are shown in Table 2.
Sample measurement results (%)
In conclusion, the method is rapid, efficient and low-toxicity, three batches of sample data show that after technological parameters are adjusted and improved, the residual quantity of ethanol in a finished product can be effectively reduced, the medication safety of people is guaranteed, the method has important significance, the analysis time is short, the inspection cost is low, more toxic and harmful reagents are not used in the method, and the method conforms to the green industrialization development trend of the pharmaceutical industry in China.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for determining the amount of ethanol in ergot maleate tablets, comprising the steps of:
respectively adding the blank solution, the reference solution and the test solution into a gas chromatograph, recording a chromatogram, and calculating the content of ethanol in the ergot maleate tablet by peak area according to an external standard method;
the chromatographic conditions are as follows:
a chromatographic column: agilent RESTEK Bef 0.32mm × 30m,0.25 μm;
temperature programming: the initial column temperature was 40 ℃, maintained for 5 minutes, heated to 150 ℃ at a rate of 10 ℃ per minute, maintained for 2 minutes, heated to 200 ℃ at a rate of 20 ℃ per minute, and maintained for 2 minutes;
sample inlet temperature: 220 ℃;
detector temperature: 250 ℃;
carrier gas: high purity nitrogen, flow rate: 3.0ml/min;
headspace bottle equilibrium temperature: 80 ℃, equilibration time: for 30 minutes.
2. The method for determining the amount of ethanol in ergot maleate tablets of claim 1, wherein the blank solution is ultra pure water.
3. The method for determining the amount of ethanol in ergot maleate tablets as claimed in claim 1, wherein the preparation of the control solution comprises: weighing 50mg of ethanol, placing the ethanol into a 100ml measuring flask, diluting the ethanol with water to a scale, shaking up, weighing 2ml of ethanol, placing the ethanol into a headspace bottle, and sealing the headspace bottle by a gland.
4. The method for determining the amount of ethanol in ergot maleate tablets as claimed in claim 1, wherein the preparation of the test solution: taking 20 tablets of the product, grinding, weighing 0.2g, placing in a 20ml headspace bottle, accurately adding 2ml of water, sealing by a gland, and shaking for 10 minutes.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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CN202211169602.0A CN115561353A (en) | 2022-09-22 | 2022-09-22 | Method for measuring amount of ethanol in ergot maleate tablets |
PCT/CN2022/138255 WO2024060426A1 (en) | 2022-09-22 | 2022-12-10 | Method for measuring ethanol content in methylergonovine maleate tablet |
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CN202211169602.0A CN115561353A (en) | 2022-09-22 | 2022-09-22 | Method for measuring amount of ethanol in ergot maleate tablets |
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CN202211169602.0A Pending CN115561353A (en) | 2022-09-22 | 2022-09-22 | Method for measuring amount of ethanol in ergot maleate tablets |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104155370A (en) * | 2013-05-13 | 2014-11-19 | 上海信谊万象药业股份有限公司 | Analytical method for determination of ethanol residual quantity in coating layer of tablet |
CN113607843A (en) * | 2021-07-30 | 2021-11-05 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | Method for detecting residual solvent in sirolimus raw material medicine |
US20220128580A1 (en) * | 2020-10-24 | 2022-04-28 | Universitatsspital Basel | Method of quantifying lysergic acid diethylamide (lsd) and 2,3-dihydro-3-hydroxy-2-oxo lysergide (o-h-lsd) in human plasma |
CN114527203A (en) * | 2021-12-31 | 2022-05-24 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | Method for detecting residual solvent in pingyangmycin hydrochloride raw material medicine |
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CN108318615A (en) * | 2018-03-16 | 2018-07-24 | 湖北亿诺瑞生物制药有限公司 | The method that headspace gas chromatography detects residual solvent in heparin sodium |
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2022
- 2022-09-22 CN CN202211169602.0A patent/CN115561353A/en active Pending
- 2022-12-10 WO PCT/CN2022/138255 patent/WO2024060426A1/en unknown
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CN104155370A (en) * | 2013-05-13 | 2014-11-19 | 上海信谊万象药业股份有限公司 | Analytical method for determination of ethanol residual quantity in coating layer of tablet |
US20220128580A1 (en) * | 2020-10-24 | 2022-04-28 | Universitatsspital Basel | Method of quantifying lysergic acid diethylamide (lsd) and 2,3-dihydro-3-hydroxy-2-oxo lysergide (o-h-lsd) in human plasma |
CN113607843A (en) * | 2021-07-30 | 2021-11-05 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | Method for detecting residual solvent in sirolimus raw material medicine |
CN114527203A (en) * | 2021-12-31 | 2022-05-24 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | Method for detecting residual solvent in pingyangmycin hydrochloride raw material medicine |
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