CN107167546A - A kind of liquid phase analysis method for the Fluconazole optical isomer that ends - Google Patents
A kind of liquid phase analysis method for the Fluconazole optical isomer that ends Download PDFInfo
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- CN107167546A CN107167546A CN201710526473.9A CN201710526473A CN107167546A CN 107167546 A CN107167546 A CN 107167546A CN 201710526473 A CN201710526473 A CN 201710526473A CN 107167546 A CN107167546 A CN 107167546A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a kind of liquid phase analysis method for the Fluconazole optical isomer that ends.The stationary phase of liquid chromatography is octadecylsilane chemically bonded silica, mobile phase is acetonitrile solution, acetonitrile concentration expressed in percentage by volume is 25 45%, L threonines and D threonines containing valid density in the acetonitrile solution, and the mol ratio of L threonines and D threonines is 24:1.The liquid phase analysis method separating effect that the present invention is provided is excellent, and without chiral chromatographic column, application cost is low, it is easy to promote.
Description
Technical field
The invention belongs to Pharmaceutical Analysis field, and in particular to a kind of liquid phase analysis method of Chinese mugwort Fluconazole optical isomer.
Background technology
End Fluconazole, entitled (2R, 3R) -2- (2,4- difluorophenyl) -3- (4- methylenepiperidines -1- the bases) -1- of chemistry
(1H-1,2,4- triazol-1-yls) -2- butanol, is first external application antifungal drug in triazole class, public by Canadian Valeant pharmacy
Department's research and development, obtain FDA approval listings, trade name Jublia on June 6th, 2014.The medicine is 10% solution, and local apply is used, mainly
For treating hand, tinea pedis as caused by Trichophyton rubrum, trichophyton gypseum, its mechanism of action is to suppress fungi 14- demethyls
Change enzyme, so as to disturb the synthesis of ergosterol.There are 2 chiral centres in the Fluconazole structure that ends, have 4 kinds of optical isomers,
In addition to the 2R/3R configurations (1) with pharmacological activity, also 2S/3S configurations (2), 2R/3S configurations (3) and 2S/3R configurations (4).
The chemical structural formula of four kinds of various configurations is as follows:
According to the associated specifications of research and development stereoisomer new drug, it is necessary to set up a set of perfect analysis method to Chinese mugwort
The optical isomer impurity of Fluconazole carries out quality control and Product Quality Evaluation.Li Peijie is provided 4 in a kind of Chinese mugwort Fluconazole
The HPLC assay methods (Chinese Journal of Pharmaceuticals, 2016,47) of optical isomer are planted, but this method uses chiral color
Compose post (Daicel Chiralpak IC chiral columns).It is well known that chiral chromatographic column is costly, and service life is short, uses
The liquid phase analysis method of chiral chromatographic column exploitation has higher application cost.
The content of the invention
It is an object of the invention to provide a kind of liquid phase point for being more economically separated analysis Chinese mugwort Fluconazole and its isomers
Analysis method.
The present invention is achieved by following technical scheme:
A kind of liquid phase analysis method for the Fluconazole optical isomer that ends, the stationary phase of liquid chromatography is octadecylsilane
Bonded silica gel, mobile phase is acetonitrile solution, and acetonitrile concentration expressed in percentage by volume is containing effective in 25-45%, the acetonitrile solution
The mol ratio of the L-threonine and D-Thr of concentration, L-threonine and D-Thr is 2-4:1.
Preferably, L-threonine, D-Thr mol ratio are 3:1.
Preferably, the L-threonine, the molar concentration sum of D-Thr are 0.3-0.5 μm of ol/L.
Preferably, described liquid phase analysis method includes following chromatographic parameter:
Chromatographic column:Octadecylsilane chemically bonded silica (C18) chromatographic column;
Mobile phase A phase:25% acetonitrile solution, L-threonine, D-Thr are respectively 0.3 μm of ol/L, 0.1 μm of ol/L;
Mobile phase B phase:45% acetonitrile solution, L-threonine, D-Thr are respectively 0.3 μm of ol/L, 0.1 μm of ol/L;
Elution program:0-5min, 0%B phase;5-8min, 0% → 50%B phase;8-10min, 50% → 100%B phase;10-
25min, 100%B phase;Flow velocity:0.7-0.9mL/min;
Column temperature:33-37℃;
Detection wavelength:208-212nm.
Preferably, flow velocity is 0.8mL/min.
Preferably, column temperature is 35 DEG C.
Preferably, Detection wavelength is 210nm.
Preferably, the specification of octadecylsilane chemically bonded silica chromatographic column is long 250mm, internal diameter 4.6mm, the μ of packing material size 5
m。
Preferably, the preferred Thermo Scientific of the octadecylsilane chemically bonded silica chromatographic columnTM AcclaimTM
120 C18。
Advantages of the present invention:
The liquid phase analysis method that the present invention is provided is without chiral chromatographic column, and application cost is low, it is easy to promote.
Brief description of the drawings
Fig. 1 is Chinese mugwort Fluconazole and its chemical structural formula of isomers;
Fig. 2 is the separating effect figure that mixed reference substance solution uses the liquid phase analysis method of embodiment 1;
Fig. 3 is the separating effect figure that need testing solution uses the liquid phase analysis method of embodiment 1;
Fig. 4 is the separating effect figure that mixed reference substance solution uses the liquid phase analysis method of embodiment 2;
Fig. 5 is the separating effect figure that mixed reference substance solution uses the liquid phase analysis method of embodiment 3.
Embodiment
Technical scheme is further described with reference to specific embodiment.
The liquid phase analysis method of the Chinese mugwort Fluconazole optical isomer of embodiment 1
First, experiment material
Shimadzu LC-20A high performance liquid chromatographs;
CPA225D electronic balances (Beijing Sai Duolisi instrument systems Co., Ltd);
Chromatographic column:Thermo ScientificTM AcclaimTM120 C18;
End the self-control of Fluconazole bulk drug, Chinese mugwort Fluconazole (1) and its 2S/3S (2), 2R/3S (3), 2S/3R (4) isomers
Reference substance self-control (purity is more than 98%), the chemical structural formula of Chinese mugwort Fluconazole and its isomers is as shown in Figure 1;
D-Thr (CAS 632-20-2, lark prestige Science and Technology Ltd., purity 98%);
L-threonine (CAS 6028-28-0, Chengdu bass spy's reagent Co., Ltd, purity 99%);
Acetonitrile is chromatographically pure, and water is deionized water, and remaining reagent is that analysis is pure.
2nd, experimental method and result
1st, solution is prepared
Diluents:25% acetonitrile solution, the L-threonine containing 0.3 μm of ol/L, 0.1 μm of ol/L D-Thr.
Reference substance solution:Precision weighs 1-4 reference substance 10mg respectively, respectively puts in 100ml measuring bottles, is dissolved with diluents
And constant volume, shake up, produce the 1-4 reference substance solutions that concentration is 100 μ g/ml.
Mixed reference substance solution:1-4 reference substance solutions are mixed in equal volume, each 25 μ g/ml of concentration mixing reference substance is obtained
Solution.
Need testing solution:Precision weighs Chinese mugwort Fluconazole bulk drug 100mg, puts in 100ml measuring bottles, is dissolved with diluents
And constant volume, shake up, produce the need testing solution that concentration is 1mg/ml.
2nd, chromatographic condition
Chromatographic column:Thermo ScientificTM AcclaimTM120 C18;
Mobile phase A phase:25% acetonitrile solution, L-threonine, D-Thr are respectively 0.3 μm of ol/L, 0.1 μm of ol/L;
Mobile phase B phase:45% acetonitrile solution, L-threonine, D-Thr are respectively 0.3 μm of ol/L, 0.1 μm of ol/L;
Elution program:0-5min, 0%B phase;5-8min, 0% → 50%B phase;8-10min, 50% → 100%B phase;10-
25min, 100%B phase;Flow velocity:0.8mL/min;
Column temperature:35℃;
Detection wavelength:210nm;
Sample size:20μL.
3rd, system suitability
Precision measures 1-4 reference substance solutions and mixed reference substance solution respectively, and sample introduction is determined, and records chromatogram, and appearance is suitable
Sequence is followed successively by 1,2,3,4, and number of theoretical plate is all higher than 10000, and separating degree is all higher than 1.5, and tailing factor is respectively less than 1.15, and blank is molten
Agent not interference measurement, mixed reference substance solution chromatogram is shown in Fig. 2.
4th, linear relationship is investigated
To weigh 1-4 reference substances appropriate for precision respectively, is dissolved and diluted respectively with mobile phase, be made 0.5,5,10,20,50,
80th, 100 and 120 μ g/ml series concentration solution, sample introduction is determined.Using peak area as ordinate, concentration is abscissa, enters line
Property return, obtain regression equation.Isomers 1-4 linear relationships in above-mentioned concentration range are good, R2> 0.9999.
5th, sensitivity is investigated
It is each appropriate that precision weighs 1-4 isomer control product, plus dilution dissolves and is diluted to 4 kinds of isomers peak heights about base
3 times of line noise.As a result the minimum detectability of Isomers is each about 1.1 × 10-3μ g, sensitivity is high.
6th, average recovery is tested
Determination of recovery rates solution is prepared according to a conventional method, the rate of recovery of Isomers is calculated, and as a result proves 4 kinds of Fluconazole of Chinese mugwort
The rate of recovery of isomers (RSD < 1.5%, n=3) between 98-102%, meets the requirements.
7th, precision and stability test
Above-mentioned mixed reference substance solution and need testing solution are taken, respectively continuous sample introduction 6 times, record chromatogram.As a result RSD is equal
Less than 2.0% (n=6), show that this method precision is good.
Above-mentioned mixed reference substance solution and need testing solution are taken respectively, are placed, are entered respectively at 0,4,8,12,24h in room temperature
Sample is determined, and records chromatogram.As a result RSD of the peak area of Chinese mugwort 4 kinds of isomers of Fluconazole in 24h is respectively less than 2.0% (n=5),
Show that mixed reference substance solution room temperature places 24h stable.
8th, bulk drug is determined
Take sample appropriate, mixed reference substance solution and need testing solution are prepared as stated above, sample introduction is determined respectively, record
Chromatogram.If any miscellaneous with Isomers retention time identical in mixed reference substance solution chromatogram in need testing solution chromatogram
Mass peak, by external standard method with the content of calculated by peak area Isomers.Need testing solution chromatogram is as shown in Figure 3.In bulk drug only
2S/3R (4) isomers is only detected, its content in three batches of samples is respectively 0.04%, 0.05%, 0.04%.
The comparative example of embodiment 2, mobile phase only adds L-threonine
First, experiment material
Shimadzu LC-20A high performance liquid chromatographs;
CPA225D electronic balances (Beijing Sai Duolisi instrument systems Co., Ltd);
Chromatographic column:Thermo ScientificTM AcclaimTM120 C18;
End the self-control of Fluconazole bulk drug, Chinese mugwort Fluconazole (1) and its 2S/3S (2), 2R/3S (3), 2S/3R (4) isomers
Reference substance self-control (purity is more than 98%), the chemical structural formula of Chinese mugwort Fluconazole and its isomers is as shown in Figure 1;
L-threonine (CAS 6028-28-0, Chengdu bass spy's reagent Co., Ltd, purity 99%)
Acetonitrile is chromatographically pure, and water is deionized water, and remaining reagent is that analysis is pure.
2nd, experimental method and result
1st, solution is prepared
Diluents:25% acetonitrile solution, the L-threonine containing 0.3 μm of ol/L.
Reference substance solution:Precision weighs 1-4 reference substance 10mg respectively, respectively puts in 100ml measuring bottles, is dissolved with diluents
And constant volume, shake up, produce the 1-4 reference substance solutions that concentration is 100 μ g/ml.
Mixed reference substance solution:1-4 reference substance solutions are mixed in equal volume, each 25 μ g/ml of concentration mixing reference substance is obtained
Solution.
2nd, chromatographic condition
Chromatographic column:Thermo ScientificTM AcclaimTM120 C18;
Mobile phase A phase:25% acetonitrile solution, L-threonine is 0.3 μm of ol/L;
Mobile phase B phase:45% acetonitrile solution, L-threonine is 0.3 μm of ol/L;
Elution program:0-5min, 0%B phase;5-8min, 0% → 50%B phase;8-10min, 50% → 100%B phase;10-
25min, 100%B phase;Flow velocity:0.8mL/min;
Column temperature:35℃;
Detection wavelength:210nm;
Sample size:20μL.
3rd, system suitability
Precision measures mixed reference substance solution, and sample introduction is determined, and records chromatogram, the Fluconazole (1) that as a result ends, 2S/3S (2),
2R/3S (3), 2S/3R (4) isomers can not realize and separate two-by-two that mixed reference substance solution chromatogram is shown in Fig. 4.
The comparative example of embodiment 3, mobile phase only adds D-Thr
First, experiment material
Shimadzu LC-20A high performance liquid chromatographs;
CPA225D electronic balances (Beijing Sai Duolisi instrument systems Co., Ltd);
Chromatographic column:Thermo ScientificTM AcclaimTM120 C18;
End the self-control of Fluconazole bulk drug, Chinese mugwort Fluconazole (1) and its 2S/3S (2), 2R/3S (3), 2S/3R (4) isomers
Reference substance self-control (purity is more than 98%), the chemical structural formula of Chinese mugwort Fluconazole and its isomers is as shown in Figure 1;
D-Thr (CAS 632-20-2, lark prestige Science and Technology Ltd., purity 98%);
Acetonitrile is chromatographically pure, and water is deionized water, and remaining reagent is that analysis is pure.
2nd, experimental method and result
1st, solution is prepared
Diluents:25% acetonitrile solution, the D-Thr containing 0.1 μm of ol/L.
Reference substance solution:Precision weighs 1-4 reference substance 10mg respectively, respectively puts in 100ml measuring bottles, is dissolved with diluents
And constant volume, shake up, produce the 1-4 reference substance solutions that concentration is 100 μ g/ml.
Mixed reference substance solution:1-4 reference substance solutions are mixed in equal volume, each 25 μ g/ml of concentration mixing reference substance is obtained
Solution.
2nd, chromatographic condition
Chromatographic column:Thermo ScientificTM AcclaimTM120 C18;
Mobile phase A phase:25% acetonitrile solution, D-Thr is 0.1 μm of ol/L;
Mobile phase B phase:45% acetonitrile solution, D-Thr is 0.1 μm of ol/L;
Elution program:0-5min, 0%B phase;5-8min, 0% → 50%B phase;8-10min, 50% → 100%B phase;10-
25min, 100%B phase;Flow velocity:0.8mL/min;
Column temperature:35℃;
Detection wavelength:210nm;
Sample size:20μL.
3rd, system suitability
Precision measures mixed reference substance solution, and sample introduction is determined, and records chromatogram, the Fluconazole (1) that as a result ends, 2S/3S (2),
2R/3S (3), 2S/3R (4) isomers can not realize and separate two-by-two that mixed reference substance solution chromatogram is shown in Fig. 5.
The liquid phase analysis method that the present invention is provided is without chiral chromatographic column, and application cost is low, it is easy to promote.
Claims (9)
1. a kind of liquid phase analysis method for the Fluconazole optical isomer that ends, it is characterised in that:The stationary phase of liquid chromatography is ten
Eight alkyl silane bonded silica gels, mobile phase is acetonitrile solution, and acetonitrile concentration expressed in percentage by volume is 25-45%, the acetonitrile solution
In L-threonine and D-Thr containing valid density, the mol ratio of L-threonine and D-Thr is 2-4:1.
2. liquid phase analysis method according to claim 1, it is characterised in that:L-threonine, D-Thr mol ratio are 3:
1。
3. liquid phase analysis method according to claim 1 or 2, it is characterised in that:The L-threonine, D-Thr rub
Your concentration sum is 0.3-0.5 μm of ol/L.
4. liquid phase analysis method according to claim 3, it is characterised in that including following chromatographic parameter:
Chromatographic column:Octadecylsilane chemically bonded silica (C18) chromatographic column;
Mobile phase A phase:25% acetonitrile solution, L-threonine, D-Thr are respectively 0.3 μm of ol/L, 0.1 μm of ol/L;
Mobile phase B phase:45% acetonitrile solution, L-threonine, D-Thr are respectively 0.3 μm of ol/L, 0.1 μm of ol/L;
Elution program:0-5min, 0%B phase;5-8min, 0% → 50%B phase;8-10min, 50% → 100%B phase;10-
25min, 100%B phase;Flow velocity:0.7-0.9mL/min;
Column temperature:33-37℃;
Detection wavelength:208-212nm.
5. liquid phase analysis method according to claim 4, it is characterised in that:Flow velocity is 0.8mL/min.
6. liquid phase analysis method according to claim 4, it is characterised in that:Column temperature is 35 DEG C.
7. liquid phase analysis method according to claim 4, it is characterised in that:Detection wavelength is 210nm.
8. liquid phase analysis method according to claim 4, it is characterised in that:Octadecylsilane chemically bonded silica (C18) color
The specification for composing post is long 250mm, internal diameter 4.6mm, 5 μm of packing material size.
9. liquid phase analysis method according to claim 8, it is characterised in that:The octadecylsilane chemically bonded silica chromatogram
The preferred Thermo Scientific of postTMAcclaimTM120C18 chromatographic columns.
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Cited By (2)
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CN115792045A (en) * | 2023-01-17 | 2023-03-14 | 北京惠之衡生物科技有限公司 | Method for detecting D-threonine in insulin aspart |
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