CN107782803A - The method for detecting isopropanol residual content in the acetoacetic ester soft capsules of ω 3 - Google Patents
The method for detecting isopropanol residual content in the acetoacetic ester soft capsules of ω 3 Download PDFInfo
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Abstract
The invention discloses a kind of method of isopropanol residual content in acetoacetic ester soft capsules of detection ω 3, this method includes：Isopropanol in the acetoacetic ester soft capsules of ω 3 is detected by gas chromatography, wherein, chromatographic condition is：Chromatographic column：(the stationary phases of Agilent DB 624：The dimethyl polysiloxane of 6% cyanogen propyl group phenyl 94%)；Detector：Flame ionization ditector (FID)；Carrier gas：Helium；Injector temperature：140 degrees Celsius；Detector temperature：250 degrees Celsius；Flow rate of carrier gas：4.0 ml/min；Split ratio：10:1；Heating schedule：Kept for 5 minutes with 40 degrees Celsius, be warming up to 210 degrees Celsius with the programming rate of 40 degrees celsius/minutes, kept for 10 minutes.Thus, isopropanol residual content in the acetoacetic ester soft capsules of ω 3 can accurately be detected using this method.
Description
Technical field
The present invention relates to pharmaceutical technology field, and specifically, the present invention relates to one kind to detect in ω -3 acetoacetic ester soft capsules
The method of isopropanol residual content.
Background technology
ω -3 acetoacetic ester soft capsules are a kind of special fish oil lipid modulating agents of GlaxoSmithKline PLC research and development, at present by the U.S.
It is diet ancillary drug to reduce the triglyceride levels of adult patients that food and medicine Surveillance Authority (FDA) is the only approved.
Isopropanol is used in the production process of ω -3 acetoacetic ester soft capsules, according to ICH guides, the daily of isopropanol allows to contact gauge
Fixed limit degree is 5000ppm.The content of ω -3 acetoacetic ester soft capsules is fat-soluble, and rubber is water solubility, detects ω -3 acetoacetic esters
Need to find suitable mixed solvent during isopropanol residual content in soft capsule to dissolve ω -3 acetoacetic ester soft capsules.Thus, inspection
The method for surveying isopropanol residual content in ω -3 acetoacetic ester soft capsules need further to study.
The content of the invention
It is contemplated that at least solves one of technical problem in correlation technique to a certain extent.Therefore, the present invention
Method of one purpose in the isopropanol residual content in a kind of detection ω -3 acetoacetic ester soft capsules are proposed.
In one aspect of the invention, the present invention proposes isopropanol residual in a kind of detection ω -3 acetoacetic ester soft capsules and contained
The method of amount.According to an embodiment of the invention, this method includes：By gas chromatography in the ω -3 acetoacetic esters soft capsule
Isopropanol is detected, wherein, chromatographic condition is：Chromatographic column：Agilent DB-624 (stationary phases：6% cyanogen propyl group phenyl-
94% dimethyl polysiloxane)；Detector：Flame ionization ditector (FID)；Carrier gas：Helium；Injector temperature：140 take the photograph
Family name's degree；Detector temperature：250 degrees Celsius；Flow rate of carrier gas：4.0 ml/min；Split ratio：10:1；Heating schedule：It is Celsius with 40
Degree is kept for 5 minutes, is warming up to 210 degrees Celsius with the programming rate of 40 degrees celsius/minutes, is kept for 10 minutes.Thus, using the party
Method can accurately detect isopropanol residual content in ω -3 acetoacetic ester soft capsules.
In addition, in detection ω -3 acetoacetic ester soft capsules according to the above embodiment of the present invention isopropanol residual content method
There can also be technical characteristic additional as follows：
In some embodiments of the invention, the condition of the gas chromatography further comprises：Head-space sampler parameter
For：Ml headspace bottle equilibrium temperature：80 degrees Celsius；Quantitative loop temperature：90 degrees Celsius；Transmission line temperature：100 degrees Celsius；Gas phase circulates
Time：25 minutes；Ml headspace bottle pressing time：2 minutes；Ml headspace bottle equilibration time：10 minutes；Sample injection time：0.05 minute；Pull out pin
Time：0.5 minute.Thus, it is possible to significantly improve the degree of accuracy for measuring isopropanol residual content in ω -3 acetoacetic ester soft capsules.
In some embodiments of the invention, containing for isopropanol in the ω -3 acetoacetic esters soft capsule is determined based on following formula
Amount：
Wherein, AsplRepresent the peak area of isopropanol to be measured in gas chromatography detection collection of illustrative plates；AstdRepresent gas chromatography
Detect the peak area of isopropanol reference substance in collection of illustrative plates；WsplThe sample weighting amount of ω -3 acetoacetic esters soft capsule to be measured is represented, unit is milli
Gram；WstdThe sample weighting amount of isopropanol reference substance is represented, unit is milligram；P represents the purity of isopropanol in isopropanol reference substance, single
Position is milligram/milligram.The accurate of isopropanol residual content in ω -3 acetoacetic ester soft capsules is measured thus, it is possible to further improve
Degree.
In some embodiments of the invention, the ω -3 acetoacetic esters soft capsule is dissolved by following mixed solvent：
0.1 mol/L aqueous sulfuric acid of 10 parts by volume and the N,N-dimethylformamide of 90 parts by volume.Thus, it is possible to further carry
Height measures the degree of accuracy of isopropanol residual content in ω -3 acetoacetic ester soft capsules.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination accompanying drawings below to embodiment
Substantially and it is readily appreciated that, wherein：
Fig. 1 is the gas chromatogram of isopropanol reference substance according to an embodiment of the invention；
Fig. 2 is the gas chromatogram of ω -3 acetoacetic esters soft capsule sample to be measured according to an embodiment of the invention；
Fig. 3 is the gas chromatogram of diluent according to an embodiment of the invention；
Fig. 4 is isopropanol canonical plotting according to an embodiment of the invention.
Embodiment
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Unreceipted particular technique or condition in embodiment, according to text in the art
Offer described technology or condition or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument,
For the conventional products of acquisition purchased in market can be passed through.
In one aspect of the invention, the present invention proposes isopropanol residual in a kind of detection ω -3 acetoacetic ester soft capsules and contained
The method of amount.The method of isopropanol residual content in detection ω -3 acetoacetic ester soft capsules according to embodiments of the present invention is entered below
Row is described in detail.According to an embodiment of the invention, this method includes：
Step (1)：Prepare reference substance solution
In this step, isopropanol reference substance solution is prepared according to the following steps：(a) weigh isopropanol reference substance and be placed in dress
Have in the 100mL volumetric flasks of 5mL diluents, solution is settled to 100mL by (b) using diluent, and (c) precision measures 2.0ml should
Solution, put in 100ml volumetric flasks, solution is settled to 100mL by (d) using diluent, and solution is placed in 20mL after (e) measures constant volume
In ml headspace bottle, seal and mix immediately.
According to one embodiment of present invention, the weight for weighing isopropanol reference substance is not particularly restricted, this area skill
Art personnel can be selected according to being actually needed, and according to the specific embodiment of the present invention, weigh isopropanol reference substance
Weight can be 350mg, and inventor is by testing it was unexpectedly observed that follow-up inspection can be significantly improved by weighing the isopropanol of the weight
Survey in step and measure the degree of accuracy of isopropanol residual content in ω -3 acetoacetic ester soft capsules.
According to still a further embodiment, the species of diluent is not particularly restricted, and those skilled in the art can
It is actually needed and is selected with basis, according to the specific embodiment of the present invention, diluent can be 10 parts by weight 0.1mol/
The mixed solution of L aqueous sulfuric acids and the DMF of 90 parts by volume, inventor is by largely testing unexpectedly
Remained it was found that can further be improved using the diluent and isopropanol in ω -3 acetoacetic ester soft capsules is measured in following detection step
The degree of accuracy of content.
According to still another embodiment of the invention, measure solution after constant volume volume measure the volume of solution after constant volume can be with
For 2.0mL, isopropanol residual content in ω -3 acetoacetic ester soft capsules is measured thus, it is possible to further improve in following detection step
The degree of accuracy.
Step (2)：Prepare testing sample solution
In this step, testing sample solution is prepared according to the following steps：(d) ω -3 acetoacetic esters soft capsule 2 is taken, accurately
Weighed quality, it is placed in 200mL volumetric flasks, (e), which adds 0.1mol/L aqueous sulfuric acids, makes the outer rubber dissolving of soft capsule, and (f) adds
Enter DMF and be settled to 200mL, solution is placed in 20mL ml headspace bottles after (g) measures constant volume, is sealed immediately
And mix.
According to one embodiment of present invention, the volume for adding 0.1mol/L aqueous sulfuric acids is not particularly restricted, this
Art personnel can be selected according to being actually needed, and according to the specific embodiment of the present invention, add 0.1mol/L
The volume of aqueous sulfuric acid can be 20mL, thus, it is possible to which it is soft further to measure ω -3 acetoacetic esters in raising following detection step
The degree of accuracy of isopropanol residual content in capsule.
According to still a further embodiment, by shaking capsule must be made complete after adding 0.1mol/L aqueous sulfuric acids
Leach, it is necessary to illustrate, inventor by many experiments be surprised to find that shaking operation to measured in following detection step ω-
The degree of accuracy of isopropanol residual content has and significantly affected in 3 acetoacetic ester soft capsules, and inventor has found, can not in shaking operates
Using being ultrasonically treated or heating, ω -3 acetoacetic ester soft capsules are measured thus, it is possible to further improve in following detection step
The degree of accuracy of middle isopropanol residual content.
Step (4)：Gather isopropanol characteristic peak
In this step, the characteristic peak of isopropanol reference substance and isopropanol to be measured is gathered by gas chromatography.Specifically,
The GC conditions include：Chromatographic column：Agilent DB-624 (stationary phases：The dimethyl of 6% cyanogen propyl group phenyl -94% gathers
Siloxanes)；Detector：Flame ionization ditector (FID)；Carrier gas：Helium；Injector temperature：140 degrees Celsius；Detector
Temperature：250 degrees Celsius；Flow rate of carrier gas：4.0 ml/min；Split ratio：10:1；Heating schedule：Kept for 5 points with 40 degrees Celsius
Clock, 210 degrees Celsius are warming up to the programming rate of 40 degrees celsius/minutes, is kept for 10 minutes；And head-space sampler parameter is：
Ml headspace bottle equilibrium temperature：80 degrees Celsius；Quantitative loop temperature：90 degrees Celsius；Transmission line temperature：100 degrees Celsius；When gas phase circulates
Between：25 minutes；Ml headspace bottle pressing time：2 minutes；Ml headspace bottle equilibration time：10 minutes；Sample injection time：0.05 minute；When pulling out pin
Between：0.5 minute.Thus, it is possible to significantly improve the degree of accuracy for measuring isopropanol residual content in ω -3 acetoacetic ester soft capsules.
Inventor is by experiment it was unexpectedly observed that the chromatographic condition in detecting step can significantly affect what detection obtained
The accuracy of isopropanol residual content in ω -3 acetoacetic ester soft capsules.In view of this, inventor is therefrom determined by many experiments
Above-mentioned chromatographic condition, thus, it is possible to significantly improve the degree of accuracy for measuring isopropanol residual content in ω -3 acetoacetic ester soft capsules.
Step (5)：Determine isopropanol residual content
In this step, the content of isopropanol in the ω -3 acetoacetic esters soft capsule is determined based on following formula：
Wherein, AsplRepresent the peak area of isopropanol to be measured in gas chromatography detection collection of illustrative plates；AstdRepresent gas chromatography
Detect the peak area of isopropanol reference substance in collection of illustrative plates；WsplThe sample weighting amount of ω -3 acetoacetic esters soft capsule to be measured is represented, unit is milli
Gram；WstdThe sample weighting amount of isopropanol reference substance is represented, unit is milligram；P represents the purity of isopropanol in isopropanol reference substance, single
Position is milligram/milligram.The accurate of isopropanol residual content in ω -3 acetoacetic ester soft capsules is measured thus, it is possible to further improve
Degree.
Below with reference to specific embodiment, present invention is described, it is necessary to which explanation, these embodiments are only to describe
Property, without limiting the invention in any way.
Conventional method
Unless stated otherwise, gas chromatographic detection is carried out using following method in embodiment below：
GC conditions include：Chromatographic column：Agilent DB-624 (stationary phases：The diformazan of 6% cyanogen propyl group phenyl -94%
Based polysiloxane)；Detector：Flame ionization ditector (FID)；Carrier gas：Helium；Injector temperature：140 degrees Celsius；Inspection
Survey device temperature：250 degrees Celsius；Flow rate of carrier gas：4.0 ml/min；Split ratio：10:1；Heating schedule：5 are kept with 40 degrees Celsius
Minute, 210 degrees Celsius are warming up to the programming rate of 40 degrees celsius/minutes, is kept for 10 minutes；And head-space sampler parameter
For：Ml headspace bottle equilibrium temperature：80 degrees Celsius；Quantitative loop temperature：90 degrees Celsius；Transmission line temperature：100 degrees Celsius；Gas phase circulates
Time：25 minutes；Ml headspace bottle pressing time：2 minutes；Ml headspace bottle equilibration time：10 minutes；Sample injection time：0.05 minute；Pull out pin
Time：0.5 minute.The retention time of isopropanol is 4.78min.
Embodiment 1
In the present embodiment, inventor is prepared for isopropanol reference substance solution and has measured it according to the description of conventional method
Gas chromatogram.It is placed in specifically, accurately weighing isopropanol reference substance 350mg in the 100mL volumetric flasks equipped with 5mL diluents,
Wherein diluent is molten for 0.1 mol/L aqueous sulfuric acid of 10 parts by volume and the N,N-dimethylformamide mixing of 90 parts by volume
Liquid, is settled to 100mL with diluent and mixes, and accurately measures the 2.0ml solution, puts in 100ml volumetric flasks, with diluent constant volume
To 100mL and mixing, solution is placed in 20mL ml headspace bottles after accurately measuring 2.0mL constant volumes, is sealed and is mixed immediately, wherein
The concentration of isopropanol reference substance is 70 μ g/mL, and the gas chromatogram of isopropanol reference substance solution is as shown in figure 1, in addition, inventor
According to 6 isopropanol reference substance solutions of description parallel determination of conventional method, relative standard deviation 2.6%, instrument precision
Degree is good.
Embodiment 2
In the present embodiment, inventor is prepared for isopropanol sample solution to be measured and measured according to the description of conventional method
Its gas chromatogram.Specifically, taking ω -3 acetoacetic esters soft capsule 2, accurate weighed quality, it is placed in 200mL volumetric flasks, adds
20 milliliters of 0.1mol/L aqueous sulfuric acids make the outer rubber dissolving of soft capsule, and shaking makes soft capsule leach completely, adds N, N- diformazans
Base formamide is settled to 200mL and mixed, and solution is placed in 20mL ml headspace bottles after accurately measuring 2.0mL constant volumes, is capped immediately close
Seal and mix, wherein soft capsule content concentration is about 14mg/mL.As a result show, with reference to figure 2, isopropanol sample solution to be measured
In unknown peak do not disturb isopropanol characteristic peak, be computed, isopropanol characteristic peak theoretical cam curve is 16270, and isopropanol is special
It is 1.0 to levy peak tailing factor.
Embodiment 3
In the present embodiment, inventor has measured the gas chromatogram of diluent according to the description of conventional method, wherein dilute
Agent is released as 0.1 mol/L aqueous sulfuric acid of 10 parts by volume and the DMF mixed solution of 90 parts by volume, as a result
Show, with reference to figure 3, the chromatographic peak of diluent does not disturb the characteristic peak of isopropanol.
Embodiment 4
In the present embodiment, inventor demonstrates the precision and repeatability of conventional method.Treated specifically, inventor uses
Description replication 6 time of the 100% horizontal recovery sample solution according to conventional method is surveyed, relative standard is inclined between the result measured
Difference is 1.6%, and method precision is good.And then inventor has prepared 6 parts of isopropanol sample solutions to be measured, according to conventional method
Description difference 6 parts of isopropanol sample peak areas to be measured of parallel determination, relative standard deviation is between the result measured
2.1%, repeatability is good.In addition, inventor is used with the different chromatographic columns of model and the reagent of different lot numbers in different time
6 parts of 100% horizontal recovery sample solutions to be measured are prepared, it is to be measured different to distinguish 6 parts of parallel determination according to the description of conventional method
Propyl alcohol sample peak area, relative standard deviation is 1.1% between the result measured, and reappearance is good.
Embodiment 5
In the present embodiment, inventor has investigated line of the isopropanol in the μ g/mL concentration ranges of 1.49 μ g/mL~148.7
Property.Specifically, inventor has prepared 6 parts of isopropanol solution to be measured, concentration is respectively 1.49 μ g/mL, 14.9 μ g/mL, 44.6 μ g/
ML, 59.5 μ g/mL, 74.4 μ g/mL, 89.2 μ g/mL, 148.7 μ g/mL, then determine and treat respectively according to the description of conventional method
The peak area of isopropanol in liquid is surveyed, and concentration is mapped with peak area, obtains standard curve.As a result show, with reference to figure 4, isopropyl
Alcohol is linear good in the μ g/mL concentration ranges of 1.49 μ g/mL~148.7.
Embodiment 6
In the present embodiment, inventor has investigated the degree of accuracy of conventional method.Specifically, inventor adds in sample solution
Enter theoretical concentration (70 μ g/mL) 50%, 100% and 120% aqueous isopropanol, 3 parts of samples of each horizontal preparation, according to one
As the description of method determine its isopropanol peak area and calculate average recovery rate, the average recovery rate of 50% horizontal sample is
100.2%, the average recovery rate of 100% horizontal sample is 100.5%, and the average recovery rate of 120% horizontal sample is
100.6%, the relative standard deviation between 9 parts of varying level results is 0.7%, and the degree of accuracy is good.
Embodiment 7
In the present embodiment, inventor has investigated the durability of conventional method.Specifically, by changing in conventional method
Chromatographic column initial temperature is 40 ± 2 degrees Celsius, and change flow rate of carrier gas is 4.0 ± 0.2 ml/mins, changes injector temperature and is
140 ± 10 degrees Celsius, it is 250 ± 10 degrees Celsius and using the level of different label chromatographic columns measure 100% to change detector temperature
Solution is reclaimed, compared with the result of 100% horizontal recovery solution is surveyed in conventional method description, the absolute difference of the rate of recovery
Within 5%, the good tolerance of conventional method is as a result shown.
Embodiment 8
In the present embodiment, inventor has investigated the recovery solution of isopropanol reference substance solution and 100% horizontal sample
Stability.Specifically, by using the isopropanol reference substance solution newly prepared, isopropanol reference substance solution and 100% is horizontal
The recovery solution of sample is placed to different time points, and the peak area for then determining isopropanol respectively according to the description of conventional method obtains
To isopropanol content, and compared with the isopropanol content value of 0 hour, its absolute difference is respectively less than 10.0% in 72 hours, knot
Fruit shows that reference substance solution and sample solution are stable in 72 hours.
Embodiment 9
In the present embodiment, inventor has investigated the test limit and quantitative limit of isopropanol.Specifically, by further diluting
Isopropanol reference substance solution, the ratio of a chromatogram peak-to-peak signal and baseline noise is obtained, by the ratio 3-5 conditions of signal and noise
Under the content of isopropanol that can be detected as test limit, by signal with can be detected under the conditions of noise values 8-12 it is different
As a result the content of propyl alcohol is shown, detection is limited to 30ppm, is quantitatively limited to 100ppm, the sensitivity of instrument is good as quantitative limit.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment or example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office
Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area
Art personnel can be tied the different embodiments or example and the feature of different embodiments or example described in this specification
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (4)
1. a kind of method of isopropanol residual content in detection ω -3 acetoacetic ester soft capsules, it is characterised in that including：
Isopropanol in the ω -3 acetoacetic esters soft capsule is detected by gas chromatography, wherein, chromatographic condition is：
Chromatographic column：Agilent DB-624 (stationary phases：The dimethyl polysiloxane of 6% cyanogen propyl group phenyl -94%)；
Detector：Flame ionization ditector (FID)；
Carrier gas：Helium；
Injector temperature：140 degrees Celsius；
Detector temperature：250 degrees Celsius；
Flow rate of carrier gas：4.0 ml/min；
Split ratio：10:1；
Heating schedule：Kept for 5 minutes with 40 degrees Celsius, be warming up to 210 degrees Celsius with the programming rate of 40 degrees celsius/minutes, protect
Hold 10 minutes.
2. according to the method for claim 1, it is characterised in that the condition of the gas chromatography further comprises：
Head-space sampler parameter is：
Ml headspace bottle equilibrium temperature：80 degrees Celsius；
Quantitative loop temperature：90 degrees Celsius；
Transmission line temperature：100 degrees Celsius；
Gas phase circulation time：25 minutes；
Ml headspace bottle pressing time：2 minutes；
Ml headspace bottle equilibration time：10 minutes；
Sample injection time：0.05 minute；
Pull out the pin time：0.5 minute.
3. according to the method for claim 2, it is characterised in that determined based on following formula different in the ω -3 acetoacetic esters soft capsule
The content of propyl alcohol：
Wherein, AsplRepresent the peak area of isopropanol to be measured in gas chromatography detection collection of illustrative plates；
AstdRepresent the peak area of isopropanol reference substance in gas chromatography detection collection of illustrative plates；
WsplThe sample weighting amount of ω -3 acetoacetic esters soft capsule to be measured is represented, unit is milligram；
WstdThe sample weighting amount of isopropanol reference substance is represented, unit is milligram；
P represents the purity of isopropanol in isopropanol reference substance, and unit is milligram/milligram.
4. according to the method for claim 1, it is characterised in that the ω -3 acetoacetic esters soft capsule is molten by following mixing
Agent dissolving：0.1 mol/L aqueous sulfuric acid of 10 parts by volume and the N,N-dimethylformamide of 90 parts by volume.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110412140A (en) * | 2018-04-28 | 2019-11-05 | 人福普克药业（武汉）有限公司 | A method of measurement bexarotene soft capsule residual solvent isopropanol |
| CN110412180A (en) * | 2018-04-28 | 2019-11-05 | 人福普克药业（武汉）有限公司 | A method of measurement Nimodipine soft capsule residual solvent isopropanol |
| CN110412141A (en) * | 2018-04-28 | 2019-11-05 | 人福普克药业（武汉）有限公司 | A method of measurement amantadine hydrochloride soft capsule residual solvent isopropanol |
| CN113866292A (en) * | 2021-09-13 | 2021-12-31 | 河北威远生物化工有限公司 | Method for measuring content of o-chlorobenzyl magnesium chloride |
| CN113866292B (en) * | 2021-09-13 | 2024-03-19 | 河北威远生物化工有限公司 | Method for measuring content of o-chlorobenzyl magnesium chloride |
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