CN106872632A - A kind of RT HPLC detection method of triprolidine hydrochloride about material - Google Patents
A kind of RT HPLC detection method of triprolidine hydrochloride about material Download PDFInfo
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- CN106872632A CN106872632A CN201710179492.9A CN201710179492A CN106872632A CN 106872632 A CN106872632 A CN 106872632A CN 201710179492 A CN201710179492 A CN 201710179492A CN 106872632 A CN106872632 A CN 106872632A
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Abstract
The present invention relates to Pharmaceutical Analysis technical field, RT HPLC detection method of more particularly to a kind of triprolidine hydrochloride about material.The invention discloses the analysis method that related 6 impurity of triprolidine hydrochloride separate simultaneously：Allocation Analysis solution；Using reverse-phase chromatographic column, the mixed liquor with acid and alkali or acid and acid ammonium salt aqueous solution organic phase as mobile phase, using isocratic or gradient elution method；Machine is determined in the analytical solution that will have been configured.Analysis method of the present invention can efficiently and accurately determine various related impuritieses in triprolidine hydrochloride, so that it is guaranteed that product is quality controllable.
Description
Technical field
The present invention relates to Pharmaceutical Analysis technical field, more particularly to a kind of triprolidine hydrochloride and its degradation impurity, isomery
The reverse high-efficiency liquid chromatography method for detecting of body and process contaminants.
Background technology
Triprolidine hydrochloride, entitled (E) -2- [1- (4- aminomethyl phenyls) -3- (1- the pyrrolidinyls) -1- acrylic] pyrrole of chemistry
Pyridine, its structural formula is as follows：
It is efficiently antiallergic action of new generation that triprolidine hydrochloride (tirporlidine hydocrhloirde, TRI) is
A kind of medicine, potent H1 receptor antagonists, with antihistamine, cholinolytic and maincenter sedation, are clinically used for treating nettle
Rash, allergic rhinitis, alleviate runny nose, the symptom of sneezing caused by flu, and curative effect is good, and side reaction is slight.U.S.'s FD A approvals
Used as OTC medicines, can be applied to children, pregnant woman's allergy treatment, be a preferable antihistamine.
Alleged " relevant material (related substances) " refers in production of raw medicine process in Pharmaceutical Analysis
In the material such as initiation material, reagent, intermediate, accessory substance and the isomers brought into, it is also possible to preparation is in production, storage and transports
The special impurities such as the catabolite, polymer or the crystal transfer that are produced during defeated.About the synthesis of the species and medicine of material
Route is closely related with preparation process, and the change of any one factor of the medicine in synthesis and production process may all cause it
Species about material is different thus relative complex about the detection and control process of material.Detection about material is control
The important indicator of drug quality.
Existing document is rarely seen have triprolidine hydrochloride isomers limit test thin-layered chromatography report, there are no it
The report of his related impurities detection method.
Initiation material, reagent, intermediate, accessory substance and the isomery brought into during triprolidine hydrochloride production of raw medicine
The impurity such as body, determine that related impurities is composed：Impurity A, B, C, D, E, F, (being shown in Table 1).
Each impurity title of the triprolidine hydrochloride of table 1 and structure
The present invention provides a kind of analysis method that can separate above-mentioned impurity and triprolidine hydrochloride.
Current each national standard must not cross 2% (QP-C) (implementation i.e. hereafter using tlc determination isomer impurities
Example 1, as shown in Figure 1), the degree of accuracy and sensitivity of the method are all very low.This patent uses HPLC analysis methods, standard limitation first
For isomers must not cross 0.5%.
The content of the invention
The present invention provides a kind of highly sensitive detection method, solve by triprolidine hydrochloride characteristic peak and degradation impurity,
The problem that isomer impurities, more synthetic intermediate and process contaminants characteristic peak are separate.
Technical solution of the present invention is as follows：
The RT-HPLC detection methods of the relevant material impurities of triprolidine hydrochloride, comprise the following steps：
A) Allocation Analysis solution；
B) chromatographic condition：
Chromatographic column is reverse-phase chromatographic column, and the reverse-phase chromatographic column is selected from phenyl silane bonded silica gel chromatographic column, octadecyl
Silane group silica gel chromatographic column or eight alkyl silane bonded silica gel chromatographic columns；With acid and alkali or acid and the acid ammonium salt aqueous solution-organic
The mixed liquor of phase is mobile phase, and water phase pH scopes 2~8, described organic phase is methyl alcohol or acetonitrile；Using isocratic or gradient elution
Method, the volume ratio of the mobile phase reclaimed water phase is 60~90%；The ratio of mobile phase described in the gradient elution presses 0,20
~30,32~35,36~45min time points, water phase volume ratio is entered for 80~75%, 80~75%, 20~30%, 20~80%
Row gradient elution；
C) machine is determined on：
The analytical solution injection high performance liquid chromatograph that step a) is made is taken, chromatography is carried out, and record chromatogram.
Preferred scheme, the RT-HPLC detection methods of the relevant material impurities of triprolidine hydrochloride, comprises the following steps：
A) Allocation Analysis solution
It is water-soluble with methyl alcohol, acetonitrile single solvent or methanol-water, acetonitrile-water, methyl alcohol-acid and alkali, methyl alcohol-acid and acid ammonium salt
The mixed solution sample dissolutions such as liquid, acetonitrile-acid and alkali, acetonitrile-acid and the acid ammonium salt aqueous solution, are made analytical solution；
B) chromatographic condition
Chromatographic column is reverse-phase chromatographic column, and the reverse-phase chromatographic column is selected from phenyl silane bonded silica gel chromatographic column, octadecyl
Silane group silica gel chromatographic column or eight alkyl silane bonded silica gel chromatographic columns；
Mixed liquor with acid and alkali or acid and the acid ammonium salt aqueous solution-organic phase is as mobile phase, and water phase pH scopes 2~8 are described
Organic phase be methyl alcohol or acetonitrile；Using isocratic or gradient elution method, volume ratio is 90~60% institutes in mobile phase reclaimed water phase
State ratio described in gradient elution in mobile phase by 0,20~30,32~35,36~45min time points, water phase volume ratio is
80~75%, 80~75%, 20~30%, 20~80% carry out gradient elution；Flow velocity is 0.8-1.3ml/min；Column temperature is 25-
60 DEG C, Detection wavelength is 205-300nm；Run time 40-70min；
C) machine is determined on
The analytical solution 5-60 μ l injection high performance liquid chromatographs that step a) is made are taken, chromatography is carried out, and record color
Spectrogram.
In certain embodiments, the filler of the reverse-phase chromatographic column is phenyl silane bonded silica gel chromatographic column or octadecane
Base silane bonded silica gel chromatographic column or eight alkyl silane bonded silica gel chromatographic columns, preferably octadecylsilane chemically bonded silica chromatogram
Post.
In certain embodiments, the specification of the reverse-phase chromatographic column is：Column length is between 100mm to 300mm, chromatogram column internal diameter
Between 1mm to 10mm, particle diameter between 1 μm to 10 μm, preferably Agilent ZORBAX C18The ten of (4.6mm × 250mm, 5 μm)
Eight alkyl silane bonded silica gel chromatographic columns.
In certain embodiments, the pH 2.0-7.0 of the water phase, the preferably pH of water phase are 2.4.
In certain embodiments, the water is mutually formic acid and ammonium formate salt solution, acetic acid and ammonium acetate salt solution, ammonium hydrogen carbonate
One of water, trifluoroacetic acid-triethylamine water, trifluoroacetic acid-diethyl aqueous amine, preferably trifluoroacetic acid-triethylamine aqueous solution.
Preferably, during isocratic elution, the mobile phase reclaimed water phase volume ratio is 90~60%.In certain embodiments, institute
It is 80~60%, preferably 70% to state mobile phase reclaimed water phase volume ratio.
Preferably, the step b is that the reverse-phase chromatographic column is octadecylsilane chemically bonded silica chromatographic column, the flowing
Mutually for acid and alkali or acid and the acid ammonium salt aqueous solution and acetonitrile mixture, acid and alkali or acid and acid ammonium salt aqueous solution pH 2.4, it is described
In mobile phase acid and alkali or acid and the acid ammonium salt aqueous solution-acetonitrile 0,20,35,38min time points, water phase volume ratio be 80%,
80%th, 30%, 80% gradient elution is carried out.Preferably, reverse-phase chromatographic column described in the step b is octadecylsilane bonded silica
Glue chromatographic column, organic phase is acetonitrile in the mobile phase, and the pH of the water phase is 2.4, and in the mobile phase, water phase volume ratio is
80~65% carry out isocratic elution.
The sample is triprolidine hydrochloride bulk drug or its preparation, and the preparation is tablet, capsule, granule, eye
With preparation, nasal formulations, suppository, pill, ointment cream, paste, suction preparation, spray, aerosol, gel, dissipate
Agent, syrup, liniment, paint, plastics, tincture, patch, oral solution, implant, film, lotion, irrigation, soft extracts
Agent, plaster, distillate medicinal water, medicinal tea.
Beneficial effect：
The present invention can effectively determine the presence of various related impuritieses in triprolidine hydrochloride solution, especially realize spectrum
Triprolidine hydrochloride characteristic peak and triprolidine hydrochloride degradation impurity characteristic peak in figure, isomer impurities characteristic peak and its it is related in
The separation of mesosome, process contaminants characteristic peak.The method of the present invention can be additionally used in the relevant material of triprolidine hydrochloride preparation simultaneously
Detection.
The detection of the above method may insure the quality controllable of product.
Brief description of the drawings
The chromatogram of the method gradient elution of Fig. 1 embodiments 1；
(note：1-3 is respectively impurity C, triprolidine hydrochloride crude product, triprolidine hydrochloride in figure)
The chromatogram of the method isocratic elution of Fig. 2 embodiments 1；
(note：1-7 is respectively impurity B, A, E, triprolidine hydrochloride, C, D, F in figure)
The chromatogram of the method gradient elution of Fig. 3 embodiments 1；
(note：1-7 is respectively impurity A, B, E, triprolidine hydrochloride, C, D, F in figure)
The chromatogram of the method gradient elution of Fig. 4 embodiments 1；
(note：1-7 is respectively impurity A, B, E, triprolidine hydrochloride, C, D, F in figure).
Specific embodiment
Below in conjunction with specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.The test method of unreceipted actual conditions in the following example, generally according to normal condition or presses
According to the condition proposed by manufacturer.Unless otherwise defined, all specialties used in text and scientific words and this area skill
Meaning known to art personnel is identical.Additionally, any method similar to described content or impartial and material all can be used for this
In inventive method.Preferable implementation described in text only presents a demonstration with material and is used.
Embodiment 1
(1) instrument and chromatographic condition
Thin-layer developing cylinder, uviol lamp (254nm)
Solvent：Butanone-dimethylformamide (1:1)
(2) experimental procedure
Take triprolidine hydrochloride appropriate, dissolved with acetonitrile and be diluted to and be molten containing about triprolidine hydrochloride 10mg in every 1ml
Liquid.Take impurity C appropriate, the solution of about impure C 2mg in every 1ml is dissolved and be diluted to acetonitrile.
Each 5 μ l of above-mentioned solution are taken, is put respectively in same silica G F254On lamellae, with butanone-dimethylformamide (1:1)
It is solvent, launches, dry, puts and inspect under uviol lamp (254nm).Result is shown in accompanying drawing 1.The method determine isomers limit be
2%, scope is larger, only controls impurity C.Other process contaminants are not controlled.
Embodiment 2
(1) instrument and chromatographic condition
High performance liquid chromatograph：U3000 highly effective liquid phase chromatographic systems and work station；
Chromatographic column：Thermo Syncronis C18The octadecylsilane chemically bonded silica color of (4.6mm × 250mm, 5 μm)
Spectrum post；
0.1% triethylamine aqueous solution is configured, trifluoroacetic acid regulation pH to 2.5 is water phase, the ratio of mobile phase reclaimed water phase-acetonitrile
Example presses 75:25 carry out isocratic degree wash-out, and setting flow velocity is 1.0ml/min, and Detection wavelength is 260nm, 30 DEG C of column temperature.
(2) experimental procedure
Triprolidine hydrochloride, impurity A, B, C, D, E, appropriate F are taken respectively, with acetonitrile-water (70:30) dissolve and be diluted to every
The mixed solution of 5 μ g each containing about triprolidine hydrochloride and impurity in 1ml, as analytical solution；
The μ l of above-mentioned analytical solution 20 are taken, liquid chromatograph is injected, chromatogram is recorded.Result is shown in accompanying drawing 2, it can be seen that this
Triprolidine hydrochloride main peak and other impurities peak are kept completely separate under part.
Embodiment 3
(1) instrument and chromatographic condition
High performance liquid chromatograph：U3000 highly effective liquid phase chromatographic systems and work station；
Chromatographic column：Phenomenex Luna C8The octadecylsilane chemically bonded silica chromatogram of (4.6mm × 250mm, 5 μm)
Post；
0.1% triethylamine aqueous solution is configured, trifluoroacetic acid regulation pH to 3.0 is water phase, the ratio of mobile phase reclaimed water phase-acetonitrile
Example is by 0,28,34,40,60min time points, water phase volume ratio carries out gradient elution for 75%, 75%, 25%, 75%, 75%,
Flow velocity 1.0ml/min；35 DEG C of column temperature, Detection wavelength 260nm；
(2) experimental procedure
Triprolidine hydrochloride, impurity A, B, C, D, E, appropriate F are taken respectively, with acetonitrile-water (70:30) dissolve and be diluted to every
The mixed solution of 10 μ g each containing about triprolidine hydrochloride and impurity in 1ml, as analytical solution；
The μ l of above-mentioned analytical solution 10 are taken, liquid chromatograph is injected, chromatogram is recorded.Result is shown in accompanying drawing 3, it can be seen that this
Nepafenac main peak and other impurities peak are kept completely separate under part.
Embodiment 4
(1) instrument and chromatographic condition
High performance liquid chromatograph：U3000 highly effective liquid phase chromatographic systems and work station
Chromatographic column：Agilent ZORBAX C18The octadecylsilane chemically bonded silica chromatogram of (4.6mm × 250mm, 5 μm)
Post
0.1% triethylamine aqueous solution is configured, trifluoroacetic acid regulation pH to 2.4 is water phase, the ratio of mobile phase reclaimed water phase-acetonitrile
Example is by 0,20,35,38,45min time points, water phase volume ratio is 80%, 80%, 30%, 80%, 80%, sets flow velocity and is
1.0ml/min, Detection wavelength is 260nm, 55 DEG C of column temperature.
(2) experimental procedure
Triprolidine hydrochloride, impurity A, B, C, D, E, appropriate F are taken respectively, with methanol-water (70:30) dissolve and be diluted to every
The mixed solution of 5 μ g each containing about triprolidine hydrochloride in 1ml, as analytical solution；
The μ l of above-mentioned analytical solution 10 are taken, liquid chromatograph is injected, chromatogram is recorded.Result is shown in accompanying drawing 3, it can be seen that this
Triprolidine hydrochloride main peak and other impurities peak are kept completely separate under part.
Each chromatographic peak separates situation
Claims (10)
1. RT-HPLC detection methods of the relevant material impurities of triprolidine hydrochloride, it is characterised in that comprise the following steps：
A) Allocation Analysis solution
B) chromatographic condition
Chromatographic column is reverse-phase chromatographic column, and the reverse-phase chromatographic column is selected from phenyl silane bonded silica gel chromatographic column, octadecylsilane
Bonded silica gel chromatographic column or eight alkyl silane bonded silica gel chromatographic columns；
With acid and alkali or acid and the acid ammonium salt aqueous solution-organic phase mixed liquor as mobile phase, water phase pH scopes 2~8, described has
Machine is mutually methyl alcohol or acetonitrile；Using isocratic or gradient elution method, mobile phase reclaimed water phase volume ratio described in the isocratic elution
Described in 90~60% the ratio of mobile phase described in gradient elution by 0,20~30,32~35,36~45min time points, water
Phase volume ratio carries out gradient elution for 80~75%, 80~75%, 20~30%, 20~80%；
C) machine is determined on
The analytical solution injection high performance liquid chromatograph that step a) is made is taken, chromatography is carried out, and record chromatogram.
2. RT-HPLC detection methods as claimed in claim 1, it is characterised in that
Step a) the Allocation Analysis solution specific steps：With methyl alcohol, acetonitrile single solvent or methanol-water, acetonitrile-water, methyl alcohol-
Acid and alkali, methyl alcohol-acid and the acid ammonium salt aqueous solution, acetonitrile-acid and alkali, acetonitrile-acid and acid ammonium salt aqueous solution mixed solution dissolving sample
Product, are made analytical solution；
Step b) the chromatographic conditions also include that flow velocity is 0.8-1.3ml/min；Column temperature is 25-60 DEG C, and Detection wavelength is 205-
300nm；Run time 40-70min.
3. RT-HPLC detection methods as claimed in claim 1 or 2, it is characterised in that the specification of the reverse-phase chromatographic column is：
, between 100mm to 300mm, between 1mm to 10mm, particle diameter is between 1 μm to 10 μm for chromatogram column internal diameter for column length.
4. RT-HPLC detection methods as claimed in claim 3, it is characterised in that the reverse-phase chromatographic column is octadecyl silicon
Alkane bonded silica gel chromatographic column, column length 250mm, chromatogram column internal diameter is 4.6mm, and particle diameter is 5 μm.
5. RT-HPLC detection methods as claimed in claim 1 or 2, it is characterised in that the pH of the water phase is 2~7, described
Acid is selected from formic acid, acetic acid, trifluoroacetic acid, glacial acetic acid, phosphoric acid, and the alkali is selected from triethylamine, diethylamine, ammoniacal liquor, the acid and acid
Ammonium salt is selected from formic acid and formic acid ammonium salt, acetic acid and acetic acid ammonium salt.
6. RT-HPLC detection methods as claimed in claim 5, it is characterised in that the water phase pH is 2.4.
7. RT-HPLC detection methods as claimed in claim 1, it is characterised in that the step b is for the reverse-phase chromatographic column
Octadecylsilane chemically bonded silica chromatographic column, the mobile phase be acid and alkali or acid and the acid ammonium salt aqueous solution and acetonitrile mixture,
Water phase pH 2.4, using gradient elution, the ratio of the mobile phase reclaimed water phase=- acetonitrile is by 0,20,35,38min time points, water
Phase volume ratio carries out gradient elution for 80%, 80%, 30%, 80%.
8. RT-HPLC detection methods as claimed in claim 1, it is characterised in that the sample is triprolidine hydrochloride raw material
Medicine or its preparation.
9. RT-HPLC detection methods as claimed in claim 8, it is characterised in that the preparation is tablet, capsule, particle
Agent, eye-drops preparations, nasal formulations, suppository, pill, ointment cream, paste, suction preparation, spray, aerosol, gel
Agent, powder, syrup, liniment, paint, plastics, tincture, patch, oral solution, implant, film, lotion, irrigation,
Soft extract, plaster, distillate medicinal water, medicinal tea.
10. the purposes of the RT-HPLC detection methods described in a kind of claim 1-9, it is characterised in that the detection method is used for
Separate following relevant material：The chemical structural formula of impurity A isThe chemical structural formula of impurity B isThe chemical structural formula of impurity C isThe chemical structural formula of impurity D isThe chemical structural formula of impurity E isThe chemical structural formula of impurity F is
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115032285A (en) * | 2021-03-08 | 2022-09-09 | 远大生命科学(武汉)有限公司 | RT-HPLC detection method for related substances of indolequinolinic acid |
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| CN1813727A (en) * | 2005-11-28 | 2006-08-09 | 陈茜 | Triprolidine hydrochloride dropping pill and its preparing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115032285A (en) * | 2021-03-08 | 2022-09-09 | 远大生命科学(武汉)有限公司 | RT-HPLC detection method for related substances of indolequinolinic acid |
| CN115032285B (en) * | 2021-03-08 | 2024-01-02 | 远大生命科学(武汉)有限公司 | RT-HPLC detection method for related substances of indoloquinolinic acid |
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