CN105929065A - Method for detecting content of ketotifen fumarate nasal drops by using liquid chromatography-mass spectrometry - Google Patents
Method for detecting content of ketotifen fumarate nasal drops by using liquid chromatography-mass spectrometry Download PDFInfo
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- CN105929065A CN105929065A CN201610259445.0A CN201610259445A CN105929065A CN 105929065 A CN105929065 A CN 105929065A CN 201610259445 A CN201610259445 A CN 201610259445A CN 105929065 A CN105929065 A CN 105929065A
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- ketotifen fumarate
- sample solution
- fumarate nasal
- nasal drop
- mass spectrometry
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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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a method for detecting the content of ketotifen fumarate nasal drops by using liquid chromatography-mass spectrometry. The objective of the invention is to provide the detection method with the advantages of accurate qualitative and quantitative performance, high efficiency, conservation of time and objective and accurate detection results. The method comprises the following successive steps: precisely weighing 1 ml of a sample solution of the ketotifen fumarate nasal drops, placing the sample solution in a measuring flask with a volume of 100 ml, adding 50% methanol to dilute the sample solution to a desired scale, allowing the diluted sample solution to pass through a filter membrane with a pore size of 0.45 [mu]m and adding filtrate into an Agilent 1290-6490 triple quadrupole liquid chromatographic-mass spectrometric instrument for detection. The method belongs to the technical field of chemical detection.
Description
Technical field
The present invention provides a kind of method detecting ketotifen fumarate nasal drop content, specifically
Say, be the method for liquid matter Series detectors ketotifen fumarate nasal drop content；Belong to chemistry inspection
Survey technology field.
Background technology
Ketotifen fumarate nasal drop is antihistamine, anti-asthmatic, has histamine H1-receptor concurrently short of money
Anti-effect and suppression anaphylaxis medium release action.It is mainly used in treating allergic rhinitis,
For department of otorhinolaryngology medication class nonprescription drugs medicine.Two receipts of " Chinese Pharmacopoeia " version in 2010
Carry.Its content assaying method is ultraviolet spectrophotometry, and this method specificity is poor.
Summary of the invention
For above-mentioned deficiency, it is an object of the invention to provide a kind of qualitative, quantitative accurate, efficiently
Save time, the method for the detection ketotifen fumarate nasal drop content that testing result is objective and accurate.
A kind of method of liquid matter Series detectors ketotifen fumarate nasal drop content, includes successively
Following step: precision takes ketotifen fumarate nasal drop sample solution 1ml and puts 100mL measuring bottle
In, add 50% methanol dilution to scale, cross the filter membrane of 0.45 micron, take filtrate detection；
Described liquid chromatograph and Mass Spectrometry Conditions
Chromatographic column: Agilent ZORBAX Eclipse Plus post 2.1 × 50mm, 1.8
μm；Mobile phase A is 0.1% formic acid, and Mobile phase B is acetonitrile, uses gradient elution program
As follows: 0-2.0min, A, 70-20%, B, 30-80%；2.0-6min, A, 20%,
B, 80%；6.-9.6min, A, 70%, B, 30%；Flow velocity 0.5ml/min；Column temperature
38℃；Sample size 2 μ l；Electrospray ionization source ESI, positive ion mode, select multiple-reaction monitoring
MRM, carrier gas temperature: 120 DEG C, carrier gas flux: 15L/min, nebulizer pressure
40psi, sheath temperature 330 DEG C, sheath throughput: 12L/min, capillary voltage 3500V,
Qualitative, quantitative ion: parent ion m/z=251.2, daughter ion m/z233.2 and m/z
205.2, collision energy is respectively 5V and 20V, Frag and is 360V.
Further, the side of above-mentioned liquid matter Series detectors ketotifen fumarate nasal drop content
Method, described described chromatograph uses Agilent1290-6490 triple level Four bar liquid phase matter
Spectrum combined instrument.
Compared with prior art, the technical scheme that the present invention provides is by the available standard of the method
True testing result, qualitative, quantitative accurately, high efficiency and time conservation, qualification result is objective and accurate,
Quality control for ketotifen fumarate nasal drop provides certain theoretical foundation.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the claim of the present invention is done the most in detail
Illustrate, but do not constitute any limitation of the invention, any in the claims in the present invention protection
The amendment of the limited number of time that scope is made, still within the claims of the present invention.
Involved in the present invention to percentage composition concentration, in addition to specified otherwise, solute is liquid
Be volumetric concentration, solute be solid be mass concentration.
Embodiment 1
A kind of method of liquid matter Series detectors ketotifen fumarate nasal drop content, includes successively
Following step: precision takes ketotifen fumarate nasal drop sample solution 1ml and puts 100mL measuring bottle
In, add 50% methanol dilution to scale, cross the filter membrane of 0.45 micron, take filtrate detection；
Described chromatograph uses the combination of Agilent1290-6490 triple level Four bar liquid chromatography mass spectrometric
Instrument.
Described liquid chromatograph and Mass Spectrometry Conditions
Chromatographic column: Agilent ZORBAX Eclipse Plus post 2.1 × 50mm, 1.8
μm；Mobile phase A is 0.1% formic acid, and Mobile phase B is acetonitrile, uses gradient elution program
As follows: 0-2.0min, A, 70-20%, B, 30-80%；2.0-6min, A, 20%,
B, 80%；6.-9.6min, A, 70%, B, 30%；Flow velocity 0.5ml/min；Column temperature
38℃；Sample size 2 μ l；Electrospray ionization source ESI, positive ion mode, select multiple-reaction monitoring
MRM, carrier gas temperature: 120 DEG C, carrier gas flux: 15L/min, nebulizer pressure
40psi, sheath temperature 330 DEG C, sheath throughput: 12L/min, capillary voltage 3500V,
Qualitative, quantitative ion: parent ion m/z=251.2, daughter ion m/z233.2 and m/z
205.2, collision energy is respectively 5V and 20V, Frag and is 360V.
Taking same batch sample 3 parts, the method worked out by the application measures, and records fumaric acid ketone
It is 2.02mg.ml for fragrant average content-1, RSD is respectively 0.2%.
The accurate ketotifen fumarate nasal drop sample (fumaric acid drawing 1ml known content
The average content of ketotifen is 2.06mg.ml-1) in 100ml volumetric flask, totally 9 parts, with 3
Part is one group, and precision adds ketotifen fumarate reference substance solution 1.199mg.ml respectively-1,
1.507mg.ml-1, 1.810mg.ml-1Each 1mL, by above-mentioned chromatographic condition sample introduction, meter
Calculate average recovery rate 99.8%, RS, 1.12%
According to two method (ultraviolet spectrophotometry) result of calculations of 2010 editions pharmacopeia with
This method results contrast, see table:
| Sequence number | Two methods of 2010 editions pharmacopeia | This method |
| 1 | 99.9% | 100% |
| 2 | 99.5% | 99.6% |
| 3 | 100% | 100% |
Claims (2)
1. a method for liquid matter Series detectors ketotifen fumarate nasal drop content, its feature
It is, comprises the steps: that precision takes ketotifen fumarate nasal drop sample solution successively
1ml puts in 100mL measuring bottle, adds 50% methanol dilution to scale, the filter of 0.45 micron excessively
Film, takes filtrate detection；
Described liquid chromatograph and Mass Spectrometry Conditions
Chromatographic column: Agilent ZORBAX Eclipse Plus post 2.1 × 50mm, 1.8
μm；Mobile phase A is 0.1% formic acid, and Mobile phase B is acetonitrile, uses gradient elution program
As follows: 0-2.0min, A, 70-20%, B, 30-80%；2.0-6min, A, 20%,
B, 80%；6.-9.6min, A, 70%, B, 30%；Flow velocity 0.5ml/min；Column temperature
38℃；Sample size 2 μ l；Electrospray ionization source ESI, positive ion mode, select multiple-reaction monitoring
MRM, carrier gas temperature: 120 DEG C, carrier gas flux: 15L/min, nebulizer pressure
40psi, sheath temperature 330 DEG C, sheath throughput: 12L/min, capillary voltage 3500V,
Qualitative, quantitative ion: parent ion m/z=251.2, daughter ion m/z233.2 and m/z
205.2, collision energy is respectively 5V and 20V, Frag and is 360V.
Liquid matter Series detectors ketotifen fumarate nasal drop the most according to claim 1 contains
The method of amount, it is characterised in that described described chromatograph uses Agilent1290-6490
Triple level Four bar liquid chromatography mass spectrometric combined instruments.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610259445.0A CN105929065A (en) | 2016-04-25 | 2016-04-25 | Method for detecting content of ketotifen fumarate nasal drops by using liquid chromatography-mass spectrometry |
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|---|---|---|---|
| CN201610259445.0A CN105929065A (en) | 2016-04-25 | 2016-04-25 | Method for detecting content of ketotifen fumarate nasal drops by using liquid chromatography-mass spectrometry |
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| CN105929065A true CN105929065A (en) | 2016-09-07 |
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| CN201610259445.0A Pending CN105929065A (en) | 2016-04-25 | 2016-04-25 | Method for detecting content of ketotifen fumarate nasal drops by using liquid chromatography-mass spectrometry |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104965038A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase microextraction-GC-MS |
| CN104965035A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS |
-
2016
- 2016-04-25 CN CN201610259445.0A patent/CN105929065A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104965038A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase microextraction-GC-MS |
| CN104965035A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS |
Non-Patent Citations (3)
| Title |
|---|
| FERAS Q. ALALI ET AL: "Determination of ketotifen in human plasma by LC-MS", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 王晓丽 等: "富马酸酮替芬颗粒与富马酸酮替芬片在健康人体的生物等效性", 《中国临床药理学杂志》 * |
| 陈江涛 等: "反相高效液相色谱法测定富马酸酮替芬滴鼻液的含量", 《药物鉴定》 * |
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Application publication date: 20160907 |