CN105203658B - The detection method of residual solvent in a kind of Ezetimibe - Google Patents
The detection method of residual solvent in a kind of Ezetimibe Download PDFInfo
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- CN105203658B CN105203658B CN201510588821.6A CN201510588821A CN105203658B CN 105203658 B CN105203658 B CN 105203658B CN 201510588821 A CN201510588821 A CN 201510588821A CN 105203658 B CN105203658 B CN 105203658B
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Abstract
In a kind of Ezetimibe, the detection method of residual solvent, belongs to technical field of analytical chemistry, and using gas chromatography, detection process is as follows：（1）The preparation of reference substance solution：Take isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid is each appropriate, accurately weighed, plus dmso solution diluting makes in every 1mL 0.5mg containing isopropanol, dichloromethane 0.06mg respectively, normal hexane 0.029mg, ethyl acetate 0.5mg, the mixed solution of acetic acid 0.5mg, used as reference substance solution；（2）The preparation of need testing solution：Ezetimibe sample 1.0g is taken, accurately weighed, put in 10mL measuring bottles, plus dmso solution be diluted to scale, shake up, as need testing solution；（3）Determine：Precision measures need testing solution and each 1 μ L of reference substance solution, injects gas chromatograph, records chromatogram, calculates content by external standard method, and each peak-to-peak separating degree all should meet the requirements.
Description
Technical field
The invention belongs to analytical chemistry field, the detection method of residual solvent in more particularly to a kind of Ezetimibe.
Background technology
Residual solvent in medicine refer to crude drug, preparation production used in be but not completely removed organic molten
Agent.If it exceeds safety value, then can affect to patient's human body, therefore drug residue is molten for the residual quantity of organic solvent
Agent has strict restriction.In the guideline of International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human use, will commonly use in pharmaceutical production
Solvent be divided into 4 classes according to the extent of injury, and define the limit value of every kind of solvent.Attached according to Chinese Pharmacopoeia version two in 2010
Record the synthesis technique of residual solvent levels requirement and Ezetimibe specified in VIII P residual solvent algoscopys, it is necessary to which control is according to folding
The organic solvent isopropanol that wheat cloth is used in synthesis technique（3rd class solvent）, dichloromethane（Equations of The Second Kind solvent）, normal hexane
（Equations of The Second Kind solvent）, ethyl acetate（3rd class solvent）, acetic acid（3rd class solvent）Residual quantity, limit is respectively：Isopropanol,
Ethyl acetate, the limit of acetic acid are 0.5%, and the limit of dichloromethane is 0.06%, and the limit of normal hexane is 0.029%.
Content of the invention
The technical problem to be solved is to provide a kind of detection method of residual solvent in Ezetimibe, utilizes
Gas chromatography is while detect the isopropanol in Ezetimibe crude drug, dichloromethane, normal hexane, ethyl acetate and acetic acid 5
Middle Determination of Residual Organic Solvents.
The gas chromatography continuous mode is as follows：
1）The preparation of reference substance solution：Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurate
Weighed, plus dmso solution diluting makes in every 1mL 0.5mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane
0.029mg, ethyl acetate 0.5mg, the mixed solution of acetic acid 0.5mg, used as reference substance solution；
2）The preparation of need testing solution：Ezetimibe sample 1.0g is taken, accurately weighed, put in 10mL measuring bottles, plus dimethyl
Sulfoxide dissolves and is diluted to scale, shakes up, used as need testing solution；
3）Determine：Precision measures 1 μ L of reference substance solution, injects gas chromatograph, records chromatogram, each peak-to-peak separating degree
All should meet the requirements.Precision measures need testing solution and each 1 μ L of reference substance solution, injects gas chromatograph, records chromatogram, presses
External standard method is with calculated by peak area；
Computing formula：Content（%）=×100%
Wherein：CRight：Isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid reference substance solution concentration, mg/mL；
CSample：Need testing solution concentration, mg/mL；
ARight：Isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid reference substance solution main peak area；
ASample：Isopropanol in need testing solution, dichloromethane, normal hexane, ethyl acetate, the peak area of acetic acid；
Wherein, chromatographic condition is：Chromatographic column：- 95% dimethyl polysiloxane of 5% diphenyl be fixing phase, 30m ×
0.53mm × 2.65 μm HP-5 capillary columns；Column temperature is temperature programming：45 DEG C of initial temperature, maintain 5 minutes, then with per point
The ramp that 10 DEG C of clock is to 100 DEG C, then with 50 DEG C per minute of ramp to 230 DEG C, maintains 5 minutes；Injector temperature
230℃；Flame ionization ditector, 250 DEG C of detector temperature, input mode are direct injected, and carrier gas is N2, flow rate of carrier gas
For 4.0mL/min.
The present invention is mainly characterized by：By the preferred of chromatographic condition, establish residue isopropanol in Ezetimibe, two
The detection method of chloromethanes, normal hexane, ethyl acetate and acetic acid, the set up method specificity of test proof is good, test limit is low,
Linear relationship, repeatability and accuracy are good.
Description of the drawings
Fig. 1：Isopropanol peak location test gas chromatogram（1. isopropanol；2. dimethyl sulfoxide）；
Fig. 2：Dichloromethane peak location test gas chromatogram（1. dichloromethane；2. dimethyl sulfoxide）；
Fig. 3：Normal hexane peak location test gas chromatogram（1. normal hexane；2. dimethyl sulfoxide）；
Fig. 4：Ethyl acetate peak location test gas chromatogram（1. ethyl acetate；2. dimethyl sulfoxide）；
Fig. 5：Acetic acid peak location test gas chromatogram（1. acetic acid；2. dimethyl sulfoxide）；
Fig. 6：The peak location test gas chromatogram of mixed reference substance solution（1. isopropanol；2. dichloromethane；3. just oneself
Alkane；4. ethyl acetate；5. acetic acid；6. dimethyl sulfoxide）.
Specific embodiment
Instrument：Japanese Shimadzu gas chromatograph（Model：GC-2014C, work station：Shimadzu）、Agilent HP-5
(30m × 0.530mm, 2.65 μm of thickness) capillary chromatographic column（Or the chromatographic column that polarity is close）, reagent is chromatographically pure.
Embodiment 1
The detection method of residual solvent in a kind of Ezetimibe, detects Ezetimibe raw material simultaneously using gas chromatography
Determination of Residual Organic Solvents in isopropanol, dichloromethane, normal hexane, ethyl acetate and acetic acid 5 in medicine,
The gas chromatography continuous mode is as follows：
4）The preparation of reference substance solution：Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurate
Weighed, plus dmso solution diluting makes in every 1mL 0.5mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane
0.029mg, ethyl acetate 0.5mg, the mixed solution of acetic acid 0.5mg, used as reference substance solution；
5）The preparation of need testing solution：Ezetimibe sample 1.0g is taken, accurately weighed, put in 10mL measuring bottles, plus dimethyl
Sulfoxide dissolves and is diluted to scale, shakes up, used as need testing solution；
6）Determine：Precision measures 1 μ L of reference substance solution, injects gas chromatograph, records chromatogram, each peak-to-peak separating degree
All should meet the requirements.Precision measures need testing solution and each 1 μ L of reference substance solution, injects gas chromatograph, records chromatogram, presses
External standard method is with calculated by peak area；
Wherein, chromatographic condition is：- 95% dimethyl polysiloxane of 5% diphenyl is chromatographic column for the capillary column of fixative；
45 DEG C of initial temperature, maintains 5 minutes；Then with 10 DEG C per minute of ramp to 100 DEG C；Again with 50 DEG C per minute of speed
230 DEG C are warming up to, are maintained 5 minutes；230 DEG C of injector temperature；250 DEG C of detector temperature, precision measure 1 μ L of reference substance solution,
Injection gas chromatograph, records chromatogram, and each peak-to-peak separating degree all should meet the requirements.Precision measures need testing solution and compares
The each 1 μ L of product solution, inject gas chromatograph, record chromatogram, by external standard method with calculated by peak area.Input mode is directly to enter
Sample, carrier gas are N2, flow rate of carrier gas is 4.0mL/min.
Method validation：
1. peak is positioned and system suitability
1.1 peak location tests
Blank solution：Dimethyl sulfoxide
Precision weighs isopropanol about 125mg, puts in 10mL measuring bottles, plus dmso solution diluting is made in every 1mL
Containing about the solution of 12.5mg, as isopropanol storing solution, precision measures isopropanol storing solution 1mL, puts in 25mL measuring bottles, plus diformazan
Base sulfoxide is diluted to scale, shakes up, and positions solution as isopropanol；
Precision weighs dichloromethane about 15mg, puts in 10mL measuring bottles, plus dmso solution diluting is made in every 1mL
Containing about the solution of 1.5mg, as dichloromethane storing solution, precision measures dichloromethane storing solution 1mL, puts in 25mL measuring bottles, plus
Dimethyl sulfoxide is diluted to scale, shakes up, and positions solution as dichloromethane；
Precision weighs normal hexane about 7.25mg, puts in 10mL measuring bottles, plus dmso solution diluting is made in every 1mL
Containing about the solution of 0.725mg, as normal hexane storing solution, precision measures normal hexane storing solution 1mL, puts in 25mL measuring bottles, plus two
Methyl sulfoxide is diluted to scale, shakes up, and positions solution as normal hexane；
Precision weighs ethyl acetate about 125mg, puts in 10mL measuring bottles, plus dmso solution dilutes and make every 1mL
In solution containing about 12.5mg, used as ethyl acetate storing solution, precision measures toluene storing solution 1mL, puts in 25mL measuring bottles, plus two
Methyl sulfoxide is diluted to scale, shakes up, and positions solution as ethyl acetate；
Precision weighs acetic acid about 125mg, puts in 10mL measuring bottles, plus dmso solution diluting is made in every 1mL about
Solution containing 12.5mg, used as acetic acid storing solution, precision measures acetic acid storing solution 1mL, puts in 25mL measuring bottles, plus dimethyl sulfoxide
Scale is diluted to, is shaken up, solution is positioned as acetic acid；
Precision measures isopropanol storing solution respectively, dichloromethane storing solution, normal hexane storing solution, ethyl acetate storing solution,
The each 1mL of acetic acid storing solution, puts in same 25mL measuring bottles, plus dimethyl sulfoxide is diluted to scale, shakes up, molten as mixing reference substance
Liquid；
This product about 1.0g is taken, accurately weighed, put in 10mL measuring bottles, plus dmso solution be diluted to scale, shake up,
As need testing solution；
Determine：Precision measures blank solution, isopropanol positioning solution, and dichloromethane positions solution, and normal hexane positions solution,
Ethyl acetate positions solution, acetic acid positioning solution positioning solution, mixed reference substance solution, each 1 μ L direct injected of need testing solution
Tested（Gas chromatogram is as shown in 1 ~ 6）, as seen from the figure：Blank solvent is to isopropanol, dichloromethane, normal hexane, acetic acid
Ethyl ester, the detection of acetic acid is noiseless, and each residual solvent chromatographic peak is met the requirements with the separating degree of adjacent chromatographic peak, isopropyl
Alcohol, dichloromethane, normal hexane, ethyl acetate, the number of theoretical plate of acetic acid peak area are all higher than 5000, illustrate that the method system is suitable for
Property is good.
1.2 system suitability
Take above-mentioned 6 pin of mixed reference substance solution continuous sample introduction, the theoretical cam curve at each peak should be greater than 5000, each peak-to-peak
Separating degree should be greater than 1.5, and the relative standard deviation of peak area must not cross 10.0%, and the RSD of each peak retention time cannot be greater than
2.0%.
2. quantitative limit
Take each positioning solution under specificity item respectively in right amount, to be placed in same measuring bottle, progressively diluted with dimethyl sulfoxide, enter
Sample is tested, and records chromatogram, and to isopropanol, dichloromethane, normal hexane, ethyl acetate, the signal to noise ratio at each peak of acetic acid are 10:1.
6 pin of continuous sample introduction, the relative standard deviation of peak area must not cross 10.0%, and the RSD of retention time cannot be greater than 2.0%, test
As a result as shown in table 1.
Table 1
3. test limit
Quantitative limit solution 3mL is taken, is put in 10mL measuring bottles, scale is diluted to dimethyl sulfoxide, shake up, sample introduction is tested, survey
Test result is as shown in table 2.
Table 2
4. linear relationship
Precision measures isopropanol storing solution, dichloromethane storing solution, normal hexane storing solution, ethyl acetate storing solution, acetic acid
Storing solution each 1.5mL, 1.0mL, 0.8mL, 0.6mL, 0.2mL, respectively put in same 25mL measuring bottles, plus dimethyl sulfoxide is diluted to quarter
Degree, shakes up, and carries out linear regression analyses with peak area and concentration, and test result is as shown in table 3.
Table 3
5. precision
5.1 it is repeated
Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurately weighed, plus dimethyl sulfoxide is molten
Solve and dilute and make in every 1mL 0.5mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane 0.029mg, ethyl acetate
0.5mg, the mixed reference substance solution of acetic acid 0.5mg, used as reference substance solution.
This product about 1.0g is taken, accurately weighed, put in 10ml measuring bottles, plus dmso solution be diluted to scale, shake up,
As need testing solution；6 parts of need testing solutions are prepared with method（Concentration all same）.
Determine：Precision measures 1 μ L of each solution, is injected separately into gas chromatograph, records chromatogram, and 6 parts of need testing solutions are equal
Isopropanol, dichloromethane, acetic acid are not detected；Normal hexane content is 0% for 0.001%, RSD；Ethyl acetate content is 0.005%,
RSD is 0%, illustrates that replica test is good.
Computing formula：C%=×100%
Wherein：CRight：Isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid reference substance solution concentration, mg/ml
CSample：Need testing solution concentration, mg/ml
ARight：Isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid reference substance solution main peak area
ASample：Isopropanol in need testing solution, dichloromethane, normal hexane, ethyl acetate, the peak area of acetic acid
5.2 Intermediate precision
By different analysts in different time operations.
Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurately weighed, plus dimethyl sulfoxide is molten
Solve and dilute and make in every 1mL 0.5mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane 0.029mg, ethyl acetate
0.5mg, the mixed reference substance solution of acetic acid 0.5mg, used as reference substance solution.
This product about 1.0g is taken, accurately weighed, put in 10mL measuring bottles, plus dmso solution be diluted to scale, shake up,
As need testing solution；6 parts of need testing solutions are prepared with method（Concentration all same）.
Determine：Precision measures 1 μ L of each solution, is injected separately into gas chromatograph, records chromatogram.And by result of calculation and weigh
Renaturation result of the test collects contrast, conclusion：Different analysis personnel are measured to this product with same instrument, and 6 parts of test samples are molten
Liquid does not detect isopropanol, dichloromethane, acetic acid；Normal hexane content is 0% for 0.001%, RSD；Ethyl acetate content is
0.005%, RSD are 0%, illustrate that the Intermediate precision of the method is good.
Computing formula：C%=×100%
Wherein：CRight：Isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid reference substance solution concentration, mg/ml
CSample：Need testing solution concentration, mg/ml
ARight：Isopropanol, dichloromethane, normal hexane, ethyl acetate, acetic acid reference substance solution main peak area
ASample：Isopropanol in need testing solution, dichloromethane, normal hexane, ethyl acetate, the peak area of acetic acid
In this experiment, 12 parts of need testing solutions do not detect isopropanol, dichloromethane, acetic acid；Normal hexane content is
0.001%, RSD are 0%；It is 0% that ethyl acetate content is 0.005%, RSD, illustrates that the method precision is good.
6. accuracy
Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurately weighed, plus dimethyl sulfoxide is molten
Solve and dilute and make in every 1mL 0.5mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane 0.029mg, ethyl acetate
0.5mg, the mixed reference substance solution of acetic acid 0.5mg, used as reference substance solution.
This product about 1.0g is taken, accurately weighed, put in 10mL measuring bottles, be separately added into quantitative limit, limit（Limit is and this part
Reference substance solution concentration is identical）Make to dissolve with the solution of 1.25 times of limit concentration and be diluted to scale, shake up, as basic, normal, high
The need testing solution of three concentration ranges, each concentration prepare 3 parts respectively.
Determine：Precision measures 1 μ L of each solution, is injected separately into gas chromatograph, records chromatogram.Determine which respectively to survey
Amount, is compared with theoretical addition amount, calculates the response rate, as a result as shown in table 4.
Computing formula：Response rate %=（Measured amount-original amount）/ addition × 100%
4 accuracy test result of table
7. ruggedness
Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurately weighed, plus dimethyl sulfoxide is molten
Solve and dilute and make in every 1mL 0.5mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane 0.029mg, ethyl acetate
0.5mg, the mixed reference substance solution of acetic acid 0.5mg, used as reference substance solution.
This product about 1.0g is taken, accurately weighed, put in 10mL measuring bottles, plus dmso solution be diluted to scale, shake up,
As need testing solution；
In the case where other conditions are constant, change injector temperature（Respectively 225 DEG C and 235 DEG C）, detector temperature
（Respectively 245 DEG C and 255 DEG C）, different in flow rate（Respectively 3.6mL/min and 4.4mL/min）, different split ratios（Respectively
18:1 and 22:1）.
Determine：Precision measures need testing solution and each 1 μ L of reference substance solution, is injected separately into gas chromatograph, records chromatograph
Figure, as a result：When chromatographic condition has less variation, system usability meets the requirements；Isopropanol, dichloromethane, acetic acid are equal
Do not detect, normal hexane content is 0% for 0.001%, RSD；It is 0% that ethyl acetate content is 0.005%, RSD, it was demonstrated that the detection method
Good tolerance.
Claims (1)
1. in a kind of Ezetimibe residual solvent detection method, it is characterised in that adopt gas chromatography, detection process is such as
Under：
（1）The preparation of reference substance solution：Isopropanol is taken, dichloromethane, normal hexane, ethyl acetate, acetic acid are each appropriate, accurate title
Fixed, plus dmso solution diluting makes in every 1mL 0.50mg containing isopropanol respectively, dichloromethane 0.06mg, normal hexane
0.029mg, ethyl acetate 0.50mg, the mixed solution of acetic acid 0.50mg, used as reference substance solution；
（2）The preparation of need testing solution：Ezetimibe sample 1.0g is taken, accurately weighed, put in 10mL volumetric flasks, plus dimethyl is sub-
Sulfone dissolves and is diluted to scale, shakes up, used as need testing solution；
（3）Determine：Precision measures need testing solution and each 1 μ L of reference substance solution, injects gas chromatograph, records chromatogram, presses
External standard method calculates content, and chromatographic condition is：Chromatographic column：- 95% dimethyl polysiloxane of 5% diphenyl be fixing phase, 30m ×
0.53mm × 2.65 μm HP-5 capillary columns；Column temperature is temperature programming：45 DEG C of initial temperature, maintain 5 minutes, then with per point
The ramp that 10 DEG C of clock is to 100 DEG C, then with 50 DEG C per minute of ramp to 230 DEG C, maintains 5 minutes；Injector temperature
230℃；Flame ionization ditector, 250 DEG C of detector temperature, input mode are direct injected, and carrier gas is N2, flow rate of carrier gas
For 4.0mL/min.
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| CN107860826B (en) * | 2016-09-22 | 2021-06-22 | 中美华世通生物医药科技(武汉)股份有限公司 | Method for measuring residual solvent in ezetimibe bulk drug by using headspace gas chromatography |
| CN107290448A (en) * | 2017-06-01 | 2017-10-24 | 广州博济医药生物技术股份有限公司 | A kind of method of residual solvent in detection memantine |
| 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 |
| CN108445110A (en) * | 2018-05-03 | 2018-08-24 | 四川科伦药业股份有限公司 | The detection method of residual solvent in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals |
| CN110208431B (en) * | 2019-07-09 | 2022-08-12 | 南京卡文迪许生物工程技术有限公司 | Method for detecting residual chloropropanol compound in medicine |
| CN112903861B (en) * | 2021-01-26 | 2022-11-15 | 山东省药学科学院 | Method for detecting residual solvent in dextral rabeprazole sodium bulk drug |
| CN115060833A (en) * | 2022-08-18 | 2022-09-16 | 精华制药集团南通有限公司 | Detection method for determining residual drug in propylthiouracil by gas chromatography |
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