CN115561353A - 一种测定马来酸甲麦角片剂中乙醇量的方法 - Google Patents
一种测定马来酸甲麦角片剂中乙醇量的方法 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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- ethanol
- ergot
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- maleate
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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
Images
Classifications
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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)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211169602.0A CN115561353A (zh) | 2022-09-22 | 2022-09-22 | 一种测定马来酸甲麦角片剂中乙醇量的方法 |
| PCT/CN2022/138255 WO2024060426A1 (fr) | 2022-09-22 | 2022-12-10 | Procédé de mesure de la teneur en éthanol dans un comprimé de maléate de méthylergonovine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211169602.0A CN115561353A (zh) | 2022-09-22 | 2022-09-22 | 一种测定马来酸甲麦角片剂中乙醇量的方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115561353A true CN115561353A (zh) | 2023-01-03 |
Family
ID=84743207
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211169602.0A Pending CN115561353A (zh) | 2022-09-22 | 2022-09-22 | 一种测定马来酸甲麦角片剂中乙醇量的方法 |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN115561353A (fr) |
| WO (1) | WO2024060426A1 (fr) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155370A (zh) * | 2013-05-13 | 2014-11-19 | 上海信谊万象药业股份有限公司 | 测定片剂包衣层中乙醇残留量的分析方法 |
| CN113607843A (zh) * | 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) | 一种检测西罗莫司原料药中残留溶剂的方法 |
| 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 (zh) * | 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) | 一种盐酸平阳霉素原料药中残留溶剂的检测方法 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108318615A (zh) * | 2018-03-16 | 2018-07-24 | 湖北亿诺瑞生物制药有限公司 | 顶空气相色谱法检测肝素钠中残留溶剂的方法 |
-
2022
- 2022-09-22 CN CN202211169602.0A patent/CN115561353A/zh active Pending
- 2022-12-10 WO PCT/CN2022/138255 patent/WO2024060426A1/fr unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155370A (zh) * | 2013-05-13 | 2014-11-19 | 上海信谊万象药业股份有限公司 | 测定片剂包衣层中乙醇残留量的分析方法 |
| 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 (zh) * | 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) | 一种检测西罗莫司原料药中残留溶剂的方法 |
| CN114527203A (zh) * | 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) | 一种盐酸平阳霉素原料药中残留溶剂的检测方法 |
Non-Patent Citations (3)
| Title |
|---|
| 吴洪应 等: "顶空气相色谱法测定阿奇霉素中的有机溶剂残留量", 中国药师, vol. 16, no. 10, pages 1550 - 1552 * |
| 周娜 等: "顶空气相色谱法同时测定硫酸特布他林中10种有机溶剂残留量", 沈阳药科大学学报, no. 05 * |
| 谢嵩 等: "顶空气相色谱法测定苯甲酸阿格列汀原料药中3种有机溶剂残留量", 中国药房, no. 09 * |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2024060426A1 (fr) | 2024-03-28 |
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