CN110426472A - A kind of method of trifluoromethayl sulfonic acid ethyl ester content in measurement drug - Google Patents
A kind of method of trifluoromethayl sulfonic acid ethyl ester content in measurement drug Download PDFInfo
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- CN110426472A CN110426472A CN201910726863.XA CN201910726863A CN110426472A CN 110426472 A CN110426472 A CN 110426472A CN 201910726863 A CN201910726863 A CN 201910726863A CN 110426472 A CN110426472 A CN 110426472A
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- sulfonic acid
- ethyl ester
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N2030/025—Gas 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The present invention provides a kind of method for measuring trifluoromethayl sulfonic acid ethyl ester content in drug, belong to drug measurement techniques field, steps are as follows: S1, taking appropriate trifluoromethayl sulfonic acid ethyl ester using methylene chloride as solvent, preparation trifluoromethayl sulfonic acid ethyl ester solution is reference substance solution；Appropriate bulk pharmaceutical chemicals are taken, using methylene chloride as solvent, prepare appropriate test solution；S2, two parts of trifluoromethayl sulfonic acid ethyl ester reference substance solutions are prepared in parallel, detected through GC-MS method, obtain the peak area of trifluoromethayl sulfonic acid ethyl ester in reference substance solution respectively；S3, it takes appropriate test solution to detect through GC-MS method, obtains the peak area of test solution, the content of trifluoromethayl sulfonic acid ethyl ester in test solution is calculated with external standard method.The present invention has detection time short, and accuracy is good, and precision is high, reproducible advantage.
Description
Technical field
The invention belongs to drug measurement techniques fields, and in particular to trifluoromethayl sulfonic acid ethyl ester content in a kind of bulk pharmaceutical chemicals
Method.
Background technique
Trifluoromethayl sulfonic acid ethyl ester is the derivative of trifluoromethayl sulfonic acid, is sulphonic acids genotoxicity impurity, as chemical industry,
The intermediate of the industries such as medicine and be widely used, medicine intermediate be some chemical raw materials used in pharmaceutical synthesis process or
Chemical products.The chemical products can produce in common chemical plant, as long as reaching certain level may be used for synthesizing
Drug.A big chunk of intermediate belongs to semi-finished product, belongs to the centre of technique, it is necessary to it is processed by certain technique, that is,
It says, it is also industrial materials, rather than final products, it is therefore desirable to control its content in drug, at present not quality mark
Standard includes the content assaying method of trifluoromethayl sulfonic acid ethyl ester.
In view of the above deficiencies, now need that a kind of detection time is short, accuracy is good, precision is high, it is reproducible for surveying
Determine the method for the content of the trifluoromethayl sulfonic acid ethyl ester in bulk pharmaceutical chemicals.
Summary of the invention
The object of the present invention is to provide a kind of methods for measuring trifluoromethayl sulfonic acid ethyl ester content, have detection time short,
Accuracy is good, and precision is high, reproducible advantage.
The present invention provides the following technical solutions:
The method of trifluoromethayl sulfonic acid ethyl ester content, includes the following steps: in a kind of measurement drug
S1, take appropriate trifluoromethayl sulfonic acid ethyl ester using methylene chloride as solvent, preparing trifluoromethayl sulfonic acid ethyl ester solution is
Reference substance solution；
Appropriate bulk pharmaceutical chemicals are taken, using methylene chloride as solvent, prepare appropriate test solution；
S2, two parts of trifluoromethayl sulfonic acid ethyl ester reference substance solutions are prepared in parallel, detect through GC-MS method, compareed respectively
The peak area of trifluoromethayl sulfonic acid ethyl ester in product solution；
S3, it takes appropriate test solution to detect through GC-MS method, obtains the peak area of test solution, calculated with external standard method
The content of trifluoromethayl sulfonic acid ethyl ester in test solution.
Preferably, a method of trifluoromethayl sulfonic acid ethyl ester content in measurement drug includes the following steps: S1, takes
31.97mg trifluoromethayl sulfonic acid ethyl ester after the dissolution that adds methylene chloride, is diluted into the 10mL measuring bottle added with certain methylene chloride
Scale shakes up, as trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 1；
Precision pipettes 0.1mL trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 1 to the 100mL amount added with certain methylene chloride
In bottle, adds methylene chloride and be diluted to scale, shake up, as trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 2；
S2, respectively precision pipette the storage of 2.0mL, 1.5mL, 1.2mL, 1.0mL, 0.5mL trifluoromethayl sulfonic acid ethyl ester reference substance
Standby liquid 2 adds methylene chloride into different 10mL measuring bottles and is diluted to scale, shake up to get L-50%~L-200% limits at different levels
Strength solution；
Precision pipettes 1.0mLL-100% linear solvent, until being diluted to scale in 5mL measuring bottle with methylene chloride, shaking up, i.e.,
Obtain L-20% test solution；
S3, L-20% solution, L-50%~L-200% limit strength solutions at different levels are detected by GC-MS method, successively into
Sample measurement, using peak area as ordinate, reference substance solution concentration is that abscissa (μ g/mL) draws trifluoromethayl sulfonic acid ethyl ester standard
Curve calculates the content of trifluoromethayl sulfonic acid ethyl ester in test solution with external standard method
Preferably, the chromatographic condition of GC-MS method is as follows in S2 step and S3 step: with 6% cyanogen propyl phenyl and 94% 2
Methyl polysiloxane is that the capillary column (DB-624UI, 30m × 0.32mm × 1.8 μm) of stationary phase is chromatographic column, injection port temperature
Degree is 150 DEG C；
Temperature program is as follows: 50 DEG C are kept for 6 minutes, 3 points of operation after being warming up at 230 DEG C, 250 DEG C per minute with 30 DEG C
Clock；Carrier gas is helium, flow velocity 1.5mL/min；Sampling volume is 1 μ L；Split ratio is 20:1；Detector is mass detector,
SIM mode is selected, trifluoromethayl sulfonic acid ethyl ester selects ion for 69,99 and 109.
The beneficial effects of the present invention are:
(1) present invention selection liquid chromatogram, while trifluoromethayl sulfonic acid ethyl ester is measured using MS detector, GC-MS method
Trifluoromethayl sulfonic acid ethyl ester can be accurately positioned in content, and response is high, and specificity is strong.；
(2) present invention uses mass detector, and high sensitivity can detecte ppm grades in sample of trifluoromethayl sulfonic acid second
Ester.；
(3) present invention measures the trifluoromethayl sulfonic acid ethyl ester content in test solution, operation letter by one point external standard method
It is single, and detection method specificity is strong, accuracy is good, precision is high, reproducible, meets the technology of the quality standard research of drug
It is required that.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is 1 reference substance solution of embodiment and test solution chromatogram；
Fig. 2 is the trifluoromethayl sulfonic acid ethyl ester canonical plotting that 2 range of linearity of embodiment is investigated；
Fig. 3 is the specificity map of 5 specificity of embodiment test；
Specific embodiment
Embodiment 1
The method of trifluoromethayl sulfonic acid ethyl ester content, includes the following steps: in a kind of measurement drug
S1, trifluoromethayl sulfonic acid ethyl ester reference substance is taken, using methylene chloride as solvent, prepares the fluoroform sulphur of debita spissitudo
Acetoacetic ester reference substance solution, as reference substance solution；Bulk pharmaceutical chemicals are taken, using methylene chloride as solvent, prepare test solution；
S2, two parts of trifluoromethayl sulfonic acid ethyl ester reference substance solutions are prepared in parallel, detect through GC-MS method, compareed respectively
The peak area of trifluoromethayl sulfonic acid ethyl ester in product solution；
S3, it takes test solution to detect through GC-MS method, obtains the peak area of test solution, calculated with external standard method for examination
The content of trifluoromethayl sulfonic acid ethyl ester in product solution.
The chromatographic condition of GC-MS method are as follows: 6% cyanogen propyl phenyl and 94% dimethyl polysiloxane are the capillary of stationary phase
Column (DB-624UI, 30m × 0.32mm × 1.8 μm) is chromatographic column, and injector temperature is 150 DEG C；Temperature program: 50 DEG C keep 6
Minute, operation 3 minutes after being warming up at 230 DEG C, 250 DEG C per minute with 30 DEG C.Carrier gas is helium, flow velocity 1.5mL/min；Into
Sample volume is 1 μ L；Split ratio is 20:1；Detector is mass detector, selects SIM mode, the selection of trifluoromethayl sulfonic acid ethyl ester
Ion is 69,99 and 109.
Using the gradient increased temperature program provided in embodiment 1, GC-MS is carried out to reference substance solution and test solution respectively
Analysis, for gained chromatogram as shown in Figure 1, figure label 2 is reference substance solution, label 3 is test solution, shows fluoroform
The retention time of sulfonic acid is 6.604min.
Embodiment 2
The range of linearity for the measuring method that embodiment 1 provides is investigated
S1, it takes 31.97mg trifluoromethayl sulfonic acid ethyl ester into the 10mL measuring bottle added with certain methylene chloride, adds methylene chloride
After dissolution, adding methylene chloride is diluted to scale and shakes up, as trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 1；Precision pipettes
0.1mL trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 1 adds methylene chloride into the 100mL measuring bottle added with certain methylene chloride
It is diluted to scale, is shaken up, as trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 2；
S2, respectively precision pipette the storage of 2.0mL, 1.5mL, 1.2mL, 1.0mL, 0.5mL trifluoromethayl sulfonic acid ethyl ester reference substance
Standby liquid 2 adds methylene chloride into different 10mL measuring bottles and is diluted to scale, shake up to get L-50%~L-200% limits at different levels
Strength solution；Precision pipettes 1.0mLL-100% linear solvent, until be diluted to scale in 5mL measuring bottle with methylene chloride, shake up,
Up to L-20% test solution；
S3, L-20% solution, L-50%~L-200% limit strength solutions at different levels are detected by GC-MS method, successively into
Sample measurement, using peak area as ordinate, reference substance solution concentration is that abscissa (μ g/mL) draws trifluoromethayl sulfonic acid ethyl ester standard
Curve calculates the content of trifluoromethayl sulfonic acid ethyl ester in test solution with external standard method.
By the measuring method that embodiment 1 provides, successively sample introduction is measured, using peak area as ordinate, reference substance solution concentration
Standard curve is drawn for abscissa (μ g/mL), the result is shown in table 1, trifluoromethayl sulfonic acid ethyl ester standard curve such as Fig. 2 institutes of drafting
Show.
1 trifluoromethayl sulfonic acid ethyl ester standard curve of table
Embodiment 3
The sample-adding recovery test for the measuring method that embodiment 1 provides
By the method for sample-adding recycling, the accuracy for the measuring method that implementation 1 provides is analyzed, bulk pharmaceutical chemicals 4mg is taken,
It is accurately weighed, it is placed in 2mL measuring bottle, parallel 11 parts, takes wherein 2 parts, measure the content of the trifluoromethayl sulfonic acid ethyl ester in sample；
Wherein 3 parts are taken, respectively plus 0.1mL trifluoromethayl sulfonic acid ethyl ester stock solution 2, scale is dissolved and be diluted to methylene chloride, as
50% recovery of standard addition solution；Wherein 3 parts are taken, it is respectively plus 0.2mL trifluoromethayl sulfonic acid ethyl ester stock solution 2, molten with methylene chloride
Scale is solved and is diluted to, as 100% recovery of standard addition solution；Wherein 3 parts are taken, respectively plus 0.3mL trifluoromethayl sulfonic acid ethyl ester
Stock solution 2 dissolves with methylene chloride and is diluted to scale, as 150% recovery of standard addition solution, by the GC-MS method of embodiment 1
Measurement, the results are shown in Table 2, the results show that the trifluoromethayl sulfonic acid ethyl ester rate of recovery is 73%~83%, the rate of recovery RSD of 9 needles is
5%, show that the measuring method that embodiment 1 provides has good accuracy.
2 trifluoromethayl sulfonic acid ethyl ester rate of recovery result of table
Embodiment 4
The precision test for the measuring method that embodiment 1 provides
By the method for 100% sample-adding recycling, the precision for the measuring method that embodiment 1 provides is analyzed, original is taken
Expect medicine 4mg, it is accurately weighed, until parallel 8 parts, taking wherein 2 parts in 2mL measuring bottle, measuring the trifluoromethayl sulfonic acid ethyl ester in sample
Content.Wherein 6 parts are taken, respectively plus 0.2mL trifluoromethayl sulfonic acid ethyl ester stock solution 2, scale is dissolved and be diluted to methylene chloride,
As 100% recovery of standard addition solution, is measured by the GC-MS method of embodiment 1, the results are shown in Table 3, the results show that fluoroform sulphur
The acetoacetic ester rate of recovery is that 76~82%, 6 needle rate of recovery RSD are 3%, and it is good to show that the measuring method of the offer of embodiment 1 has
Repeatability.
The repeated result of table 3
Embodiment 5
The specificity test for the measuring method that embodiment 1 provides
Taking methylene chloride is blank solvent, and reference substance solution and each 1 μ L of test solution in embodiment 1 are injected separately into GC-
MS is measured by the GC-MS method of the present embodiment 1, is recorded chromatogram, as a result see that Fig. 3,1 blank solvent of figure label, label 2 are
Reference substance solution in embodiment 1, label 3 are the test solution in embodiment 1, the results showed that, blank solvent and test sample
Solution measures trifluoromethayl sulfonic acid ethyl ester noiseless.
Embodiment 6
The stability test for the measuring method that embodiment 1 provides.
Reference substance solution in Example 1, is placed at room temperature, stability of solution is investigated, by the GC-MS of embodiment 1
Method, sample introduction, records the peak area of trifluoromethayl sulfonic acid ethyl ester respectively, and note calculates reference substance solution peak area RSD, the results are shown in Table 4, knot
Fruit shows in 11.5h that the peak area RSD of reference substance solution is 8%, and it is good to illustrate that the measuring method of the offer of embodiment 1 has
Stability.
4 reference substance solution stability result of table
By above-mentioned data it is found that the present invention selects liquid chromatogram, while trifluoro is measured using MS detector, GC-MS method
Trifluoromethayl sulfonic acid ethyl ester can be accurately positioned in Loprazolam ethyl ester content, and response is high, and specificity is strong；Using mass detector, spirit
Sensitivity is high, can detecte ppm grades in sample of trifluoromethayl sulfonic acid ethyl ester；It is measured in test solution by one point external standard method
Trifluoromethayl sulfonic acid ethyl ester content, it is easy to operate, and detection method specificity is strong, accuracy is good, precision is high, reproducible,
Meet the technical requirements of the quality standard research of drug.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of method of trifluoromethayl sulfonic acid ethyl ester content in measurement drug, it is characterised in that: its step are as follows,
S1, take appropriate trifluoromethayl sulfonic acid ethyl ester using methylene chloride as solvent, preparing trifluoromethayl sulfonic acid ethyl ester solution is control
Product solution；
Appropriate bulk pharmaceutical chemicals are taken, using methylene chloride as solvent, prepare appropriate test solution；
S2, two parts of trifluoromethayl sulfonic acid ethyl ester reference substance solutions being prepared in parallel, being detected through GC-MS method, it is molten to obtain reference substance respectively
The peak area of trifluoromethayl sulfonic acid ethyl ester in liquid；
S3, it takes appropriate test solution to detect through GC-MS method, obtains the peak area of test solution, calculated with external standard method for examination
The content of trifluoromethayl sulfonic acid ethyl ester in product solution.
2. the method for trifluoromethayl sulfonic acid ethyl ester content in a kind of measurement drug according to claim 1, it is characterised in that:
S1, take 31.97mg trifluoromethayl sulfonic acid ethyl ester into the 10mL measuring bottle added with certain methylene chloride, add methylene chloride dissolution
Afterwards, it adds methylene chloride and is diluted to scale and shakes up, as trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 1；
Precision pipettes 0.1mL trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 1 to the 100mL measuring bottle added with certain methylene chloride
In, it adds methylene chloride and is diluted to scale, shake up, as trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 2；
S2, respectively precision pipette 2.0mL, 1.5mL, 1.2mL, 1.0mL, 0.5mL trifluoromethayl sulfonic acid ethyl ester reference substance stock solution 2
To in different 10mL measuring bottles, adds methylene chloride and be diluted to scale, shake up to get L-50%~L-200% limit concentration at different levels
Solution；
Precision pipettes 1.0mL L-100% linear solvent, until be diluted to scale with methylene chloride in 5mL measuring bottle, shake up to get
L-20% test solution；
S3, L-20% solution, L-50%~L-200% limit strength solutions at different levels are detected by GC-MS method, successively sample introduction is surveyed
Fixed, using peak area as ordinate, reference substance solution concentration is that abscissa (μ g/mL) draws trifluoromethayl sulfonic acid ethyl ester standard song
Line calculates the content of trifluoromethayl sulfonic acid ethyl ester in test solution with external standard method.
3. the method for trifluoromethayl sulfonic acid ethyl ester content, feature exist in a kind of measurement drug according to claim 1 or 2
In: the chromatographic condition of GC-MS method is as follows: using 6% cyanogen propyl phenyl and 94% dimethyl polysiloxane as the capillary of stationary phase
Column (DB-624UI, 30m × 0.32mm × 1.8 μm) is chromatographic column, and injector temperature is 150 DEG C；
Temperature program is as follows: 50 DEG C are kept for 6 minutes, operation 3 minutes after being warming up at 230 DEG C, 250 DEG C per minute with 30 DEG C；It carries
Gas is helium, flow velocity 1.5mL/min；Sampling volume is 1 μ L；Split ratio is 20:1；Detector is mass detector, selection
SIM mode, trifluoromethayl sulfonic acid ethyl ester select ion for 69,99 and 109.
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| CN112730642A (en) * | 2020-12-04 | 2021-04-30 | 深圳海王医药科技研究院有限公司 | Method for simultaneously detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in tubulin inhibitor bulk drug |
| CN112782303A (en) * | 2020-12-28 | 2021-05-11 | 上海微谱化工技术服务有限公司 | Quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in medicine |
| CN113252809A (en) * | 2021-04-25 | 2021-08-13 | 英格尔检测技术服务（上海）有限公司 | Method for detecting residues of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112730642A (en) * | 2020-12-04 | 2021-04-30 | 深圳海王医药科技研究院有限公司 | Method for simultaneously detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in tubulin inhibitor bulk drug |
| CN112730642B (en) * | 2020-12-04 | 2023-03-07 | 深圳海王医药科技研究院有限公司 | Method for simultaneously detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in tubulin inhibitor bulk drug |
| CN112782303A (en) * | 2020-12-28 | 2021-05-11 | 上海微谱化工技术服务有限公司 | Quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in medicine |
| CN112782303B (en) * | 2020-12-28 | 2022-07-12 | 上海微谱化工技术服务有限公司 | Quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in medicine |
| CN113252809A (en) * | 2021-04-25 | 2021-08-13 | 英格尔检测技术服务（上海）有限公司 | Method for detecting residues of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate |
| CN113252809B (en) * | 2021-04-25 | 2022-10-14 | 英格尔检测技术服务（上海）有限公司 | Method for detecting residues of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate |
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Application publication date: 20191108 |
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