CN107543881B - The method of quality control of phenprobamate piece - Google Patents
The method of quality control of phenprobamate piece Download PDFInfo
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- CN107543881B CN107543881B CN201710732845.3A CN201710732845A CN107543881B CN 107543881 B CN107543881 B CN 107543881B CN 201710732845 A CN201710732845 A CN 201710732845A CN 107543881 B CN107543881 B CN 107543881B
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Abstract
The invention discloses a kind of method of quality control of phenprobamate piece, the method the related quality of the pharmaceutical preparations detection method of existing phenprobamate piece there are aiming at the problem that improved, IR identification, Related substances separation, dissolution test are mainly increased, and assay is carried out using HPLC method.Method of quality control design of the invention is rationally, accurate and reliable, specificity is strong and easy to operate, the new quality control standard of phenprobamate piece is established accordingly, the production of phenprobamate piece, circulation can be helped effectively to control, using the drug quality in all links and improve its quality level, guarantee that production technology is controllable, ensure clinical use safety, stablizes for product curative effect and definitely provide reliable guarantee.
Description
Technical field
The invention belongs to technical field of medicine quality control more particularly to a kind of method of quality control of phenprobamate piece.
Background technique
Phenprobamate (Phenprobamate) is a kind of contrastimulant central skeletal muscle relaxant of tool, earliest by
Siegfried is successfully synthesized in nineteen sixty, is listed first in Japan and Germany.Tianjin Zhongxin Pharmaceutical Group Co., Ltd. in
The certification of raw material is obtained within 1981 first；The same year, Tianjin Lisheng Pharmaceutical Co., Ltd. obtain the certification of tablet.This product is in state
A kind of interior only dosage form of tablet, specification 200mg.Clinically it is usually used in the muscle such as muscle cramp, myotonia epitonos, muscle
Pain and neuralgia, it can also be used to which inflammation, rheumatic arthritis, ligament injury, myotenositis around shoulder neck joint are additionally used for youngster
The adjuvant treatment of virgin Lennox-Gastaut syndrome.
The standard of phenprobamate tablet was recorded for two in " Chinese Pharmacopoeia " nineteen ninety-five version, from version in 2000 to version in 2015
Pharmacopeia does not record the kind again, did not during which also do standard and improves work, therefore the current standard of this product is more old.External medicine
The standard preparation of the uncharged phenprobamate of allusion quotation.It is fewer with the document of the related phenprobamate raw material and tablet delivered, at present
Document related with quality standard mainly has: (1) " content of rp-hplc determination phenprobamate piece " Yu little Ping,
Zhang Zhigen；Medical Leader in August, 2005 the 8th phase of volume 24.(2) determined by ultraviolet spectrophotometry phenprobamate piece content is ground
Study carefully, Tian Yong；Tianjin pharmacy in August, 1999 the 3rd phase of volume 11.The setting of current standard detection project is simpler, and gaps and omissions is more, lacks
Quality control item in relation to key indexes such as substance, dissolution rates；Inspection item setup is unreasonable, the method for inspection is unreasonable, such as it
Content assaying method is ultraviolet spectrophotometry or nitriding, and specificity is not good enough.For this purpose, existing method is difficult to effectively control production
In final product quality, the quality of different batches of product is unable to ensure product curative effect that rationally accurately index is not measured,
Clinical treatment is influenced huge.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of designs rationally, accurate and reliable, specificity is strong and easy to operate
Phenprobamate piece method of quality control, with help effectively control phenprobamate piece production in final product quality and improve its matter
Amount is horizontal, it is ensured that clinical use curative effect.
In order to solve the above technical problems, the invention adopts the following technical scheme:
The method of quality control of phenprobamate piece, comprising the following steps:
<1>IR identifies；
<2>Related substances separation；
<3>dissolution test；
<4>HPLC method assay.
Step<1>is carried out by following operation: being taken this product fine powder appropriate, is added ethyl alcohol 20ml, grinding dissolution, filtration, water-bath steaming
It is dry, residue is taken, is measured in accordance with the law.
Step<2>is according to high effective liquid chromatography for measuring；
Chromatographic condition and system suitability
It is filler with octadecylsilane chemically bonded silica, is mobile phase with methanol-water 50: 50；Detection wavelength is
259nm；Phenprobamate reference substance about 20mg is weighed, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, is added in 70 DEG C of water-baths after mixing
Heat 30 minutes, lets cool, is neutralized to neutrality with sodium hydroxide test solution, be diluted to 20ml, as system suitability solution with mobile phase；
Precision measures 20 μ l and injects liquid chromatograph；
Measuring method
It takes this product fine powder appropriate, add flowing phased soln and is diluted in every 1ml containing about the solution of phenprobamate 2mg, shake up,
Filtration, as test solution；Precision measures in right amount, is quantitatively diluted with mobile phase and solution of every 1ml containing about 20 μ g is made, as
Contrast solution；20 μ l test solutions and contrast solution are taken, liquid chromatograph, record spectrogram to main peak retention time are injected separately into
2 times.
Step<3>is measured according to dissolution rate and drug release determination method: being taken this product, is dissolution with pH1.2 hydrochloric acid solution 900ml
Medium, revolving speed are 50 turns per minute, operate according to methods, when through 45 minutes, solution are taken to filter in right amount, discard at least 10ml primary filtrate,
Take subsequent filtrate as test solution；Another precision weighs phenprobamate reference substance 22mg, sets in 100ml measuring bottle, methanol 5ml is added to make
Dissolution, then solubilization go out medium to scale, shake up, as reference substance solution；Take above two solution according to UV-vis spectroscopy
Photometry measures absorbance at the wavelength of 260nm, calculates every the amount of dissolution.
Step<4>is according to high effective liquid chromatography for measuring；
Chromatographic condition and system suitability
It is filler with octadecylsilane chemically bonded silica, is mobile phase with methanol-water 50: 50；Detection wavelength is
259nm；Phenprobamate reference substance about 20mg is weighed, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, is added in 70 DEG C of water-baths after mixing
Heat 30 minutes, lets cool, is neutralized to neutrality with sodium hydroxide test solution, be diluted to 20ml, as system suitability solution with mobile phase；
Precision measures 20 μ l and injects liquid chromatograph；
Measuring method
This product 20 are taken, accurately weighed, finely ground, precision measurement fine powder is appropriate, is placed in 100ml volumetric flask, and flowing is added
Mutually appropriate dissolution, and it is diluted to scale, it shakes up, filters, take subsequent filtrate as test solution；Reference substance about 10mg separately is taken, essence
It is close weighed, flowing phased soln is added and quantifies the solution that the 0.4mg containing phenprobamate in every 1ml is made in dilution；Precision measures above-mentioned
Each 20 μ l of solution, is injected separately into liquid chromatograph, according to external standard method with calculated by peak area.
The related quality of the pharmaceutical preparations detection method of existing phenprobamate piece there are aiming at the problem that, inventor is improved, main
If increasing IR identification, Related substances separation, dissolution test, and assay is carried out using HPLC method.Of the invention
Method of quality control design is rationally, accurate and reliable, specificity is strong and easy to operate, establishes the new quality control of phenprobamate piece accordingly
Standard processed can help effectively to control the production of phenprobamate piece, circulation, using the final product quality in all links and improve its quality water
It is flat, guarantee that production technology is controllable, it is ensured that clinical use safety is stablized for product curative effect and definitely provides reliable guarantee.
Detailed description of the invention
Fig. 1 is phenprobamate control map (Chinese Pharmacopoeia infrared spectroscopy collection Figure 22 9).
Fig. 2 is phenprobamate reference substance infrared spectrogram.
Fig. 3 is phenprobamate piece infrared spectrogram.
Fig. 4 is the related substance chromatogram of phenprobamate.
Fig. 5 is the dissolution curve of each factory's phenprobamate piece.
Fig. 6 is the dissolution curve of the multiple batches of phenprobamate piece of B factory.
Fig. 7 is the dissolution curve of the multiple batches of phenprobamate piece of C factory.
Fig. 8 is the system suitability map of phenprobamate HPLC assay.
Fig. 9 is phenprobamate raw material typical case's map.
Figure 10 is phenprobamate piece test solution typical case's map.
Figure 11 is that three kinds of method assay results compare figure.
Specific embodiment
The method of quality control of phenprobamate piece is studied
National general bureau database is inquired, phenprobamate only has a kind of dosage form of tablet, and 1 specification is 200mg.This grinds
Study carefully and has extracted multiple producers totally 96 batch phenprobamate piece.
<1>IR identifies
By using technological means such as powder x-ray diffraction, infrared spectroscopy, near infrared spectrums, phenprobamate is compareed
Product, raw material and raw material recrystallised sample are analyzed, and do not find that three's map has differences, thus prove phenprobamate raw material
It should be single crystal form.
After phenprobamate ethyl alcohol, chloroform and water recrystallization, IR map and reference substance map compare map holding one
It causes, therefore tablet can extract measurement IR spectrum after phenprobamate with ethyl alcohol, establish the IR Hyperspectral indexes of tablet.The benzene drafted
Third urethane piece infrared spectroscopy discrimination method is as follows:
It takes this product fine powder appropriate (being approximately equivalent to phenprobamate 200mg), adds ethyl alcohol 20ml, grinding dissolution, filtration, water-bath steaming
It is dry, residue is taken, is measured in accordance with the law；The infrared absorption pattern of this product should be with the map (229 figure of Chinese Pharmacopoeia infrared spectroscopy collection) that compares
Unanimously.
Method detects each batch phenprobamate piece, gained IR map (Fig. 3, each batch result are similar) and reference substance figure like this
Spectrum (see Fig. 2), control map (see Fig. 1) are consistent.
<2>Related substances separation
In conjunction with documents and materials and experimental exploring, attempt to establish related substance in phenprobamate raw material and tablet using HPLC method
The method of inspection.Method has carried out that mobile phase investigation, the selection of Detection wavelength, solvent selection, specificity is investigated, linear relationship examines
It examines, stability of solution, sample introduction precision, detection limits and the methods of limit determines research work, the Related substances separation drafted
Method is as follows:
It is measured according to high performance liquid chromatography (Chinese Pharmacopoeia general rule 0512)；
Chromatographic condition and system suitability
It is filler with octadecylsilane chemically bonded silica, with methanol-water (50: 50) for mobile phase；Detection wavelength is
259nm；Phenprobamate reference substance about 20mg is weighed, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, is added in 70 DEG C of water-baths after mixing
Heat 30 minutes, lets cool, is neutralized to neutrality with sodium hydroxide test solution, be diluted to 20ml, as system suitability solution with mobile phase；
Precision measures 20 μ l and injects liquid chromatograph；The separating degree of phenylpropanol (relative retention time is about 0.9) and phenprobamate should accord with
It closes and requires；
Measuring method
It takes this product fine powder appropriate, add flowing phased soln and is diluted in every 1ml containing about the solution of phenprobamate 2mg, shake up,
Filtration, as test solution；Precision measures in right amount, is quantitatively diluted with mobile phase and solution of every 1ml containing about 20 μ g is made, as
Contrast solution；20 μ l test solutions and contrast solution are taken, liquid chromatograph, record spectrogram to main peak retention time are injected separately into
2 times；If any impurity peaks in test solution, single impurity peak area is not greater than 0.3 times of contrast solution main peak area
(0.3%), the sum of each impurity peak area is not greater than contrast solution main peak area (1.0%).
Using the Related substances separation method drafted, 3 batches of phenprobamate raw materials, 96 batches of phenprobamate pieces are measured,
6 kinds of impurity are detected altogether, and impurity 1~6 is successively named as by retention time.The content that each impurity detects in raw material and tablet
Range is shown in Table 1.On the whole, the amount of impurities and content detected in phenprobamate raw material and tablet is little.Impurity content point
Cloth is shown in Fig. 4.
The miscellaneous mass spectrographic ownership of 1 phenprobamate of table and content range table
Show that the impurity of phenprobamate is main through destructive testing, accelerated stability test and interpretation of mass spectra experimental study
From the production technology of raw material and tablet, amount of impurities is little, the current total impurities of raw material control 0.2% with
Under, the total impurities of tablet are controlled 0.5% hereinafter, the quality of product is preferable.Because of partial supplementary material peak and impurity peaks separating degree
Less, when considering routine check, all auxiliary materials are calculated by impurity peaks, the largest single impurity content of tablet is 0.29%, always miscellaneous to contain
Amount is 0.84%.According to the studies above as a result, in conjunction with domestic production technological level, it is horizontal to formulate the limit of impurities are as follows: phenprobamate
The single impurity of raw material must not cross 0.2%, and total impurities must not cross 0.3%；The single impurity of tablet must not cross 0.3%, miscellaneous
Matter total amount must not cross 1.0%.
<3>dissolution test
Inventor has investigated phenprobamate raw material, and in 4 kinds of dissolution mediums, (water, pH1.2 hydrochloric acid solution, pH4.0 acetate are slow
Fliud flushing and pH6.8 phosphate buffer) in dissolution rate have larger difference, dissolution rate is maximum in pH1.2 hydrochloric acid solution, therefore
It determines using pH1.2 hydrochloric acid solution as the dissolution medium of phenprobamate piece.Using water 900ml as dissolution medium, at 50 revs/min of revolving speed
Under conditions of, when most domestic producer sample was through 45 minutes, the amount of dissolution is more than the 75% of labelled amount, in conjunction with Japanese orange peel
Book determines that dissolution test revolving speed is 50 revs/min, and sample time is 45 minutes.The phenprobamate tablet dissolution inspection drafted
It is as follows:
It is measured according to dissolution rate and drug release determination method (0,931 second method of Chinese Pharmacopoeia general rule): this product is taken, with pH1.2 salt
Acid solution 900ml is dissolution medium, and revolving speed is 50 turns per minute, operates according to methods, when through 45 minutes, solution is taken to filter in right amount, abandons
At least 10ml primary filtrate is gone, takes subsequent filtrate as test solution；Another precision weighs phenprobamate reference substance 22mg, sets 100ml
In measuring bottle, methanol 5ml is added to make to dissolve, then solubilization goes out medium to scale, shakes up, as reference substance solution；It takes above two
Solution shines UV-VIS spectrophotometry, and absorbance is measured at the wavelength of 260nm, calculates every the amount of dissolution, and limit is mark
The 75% of the amount of showing should meet regulation.
The phenprobamate piece of the different batches of the phenprobamate piece and same producer of method detection different manufacturers like this, institute
Obtain dissolution curve such as Fig. 5~7.As shown in figure 5, the amount of dissolution is more than labelled amount when most domestic producer sample was through 45 minutes
75%, and batch between dissolution difference less (Fig. 6, other producers are substantially similar), it is molten but when having one product through 45 minutes
The 70% of the below standard amount of showing of output, and widely different (Fig. 7) is dissolved out between criticizing.This prompts the production technology and its stabilization of the producer
There are problems for property.
<4>HPLC method assay
In conjunction with documents and materials and experimental exploring, the HPLC content assaying method of phenprobamate raw material and tablet, allusion quotation are established
Type chromatogram is shown in Fig. 8~10.The phenprobamate piece HPLC method assay drafted is as follows:
It is measured according to high performance liquid chromatography (Chinese Pharmacopoeia general rule 0512)；
Chromatographic condition and system suitability
It is filler with octadecylsilane chemically bonded silica, with methanol-water (50: 50) for mobile phase；Detection wavelength is
259nm；Phenprobamate reference substance about 20mg is weighed, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, is added in 70 DEG C of water-baths after mixing
Heat 30 minutes, lets cool, is neutralized to neutrality with sodium hydroxide test solution, be diluted to 20ml, as system suitability solution with mobile phase；
Precision measures 20 μ l and injects liquid chromatograph；The separating degree of phenylpropanol (relative retention time is about 0.9) and phenprobamate should accord with
It closes and requires；
Measuring method
This product 20 are taken, accurately weighed, finely ground, precision measures fine powder in right amount (being equivalent to phenprobamate 40mg), is placed in
In 100ml volumetric flask, mobile phase is added and dissolves in right amount, and is diluted to scale, shakes up, filters, takes subsequent filtrate molten as test sample
Liquid；Reference substance about 10mg separately is taken, accurately weighed, addition, which flows phased soln and quantifies dilution, to be made in every 1ml containing phenprobamate
The solution of 0.4mg；Precision measures above-mentioned each 20 μ l of solution, is injected separately into liquid chromatograph, according to external standard method with calculated by peak area,
It should be the 90.0%~110.0% of labelled amount.
96 batches of samples are compared according to the content results of UV method, nitriding, Syrups by HPLC (see figure respectively
11), the HPLC method measurement result with nitriding measurement result of most of sample are closer to, and UV method is because using old lot number reference substance
Experiment, most of inspection result are relatively low.Meanwhile influence of the auxiliary material in measurement is investigated with blank auxiliary, as the result is shown: using fixed
When nitrogen method measures phenprobamate piece content, blank auxiliary is noiseless.
Measured result is analyzed with SPSS16.0 software, analysis the result shows that, between nitriding and liquid phase method
There is no significant difference, nitriding and ultraviolet method, there is significant difference between ultraviolet method and liquid phase method.
A collection of tablet samples are chosen, by nitriding, HPLC method, UV method replication 20 times, carry out method ratio with t inspection
Compared with.As the result is shown: there is significant difference (being shown in Table 2) in three kinds of methods.The wherein result ratio HPLC method measurement of nitriding measurement
Result it is high by 2.7%, it is higher by 3.5% than UV method measurement result.Wherein for UV method because of reference substance problem, measurement result is relatively low, it is not recommended that
Assay for tablet；2% range of gap mean of access allowable error between HPLC method and nitriding.
Consider from the convenience of measuring method, HPLC method is slightly better than nitriding.
Therefore, nitriding and HPLC method can Accurate Determining phenprobamate raw material and tablet contents.UV method is built vulnerable to interference
View is not used in the assay of the kind.
2 three kinds of method assay result t inspections of table are compared
Claims (4)
1. a kind of method of quality control of phenprobamate piece, it is characterised in that the following steps are included:
<1>IR identifies；
<2>Related substances separation；
Step<2>is according to high effective liquid chromatography for measuring；
Chromatographic condition and system suitability
It is filler with octadecylsilane chemically bonded silica, using methanol-water 50:50 as mobile phase；Detection wavelength is 259nm；Claim
Phenprobamate reference substance about 20mg is taken, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, heats 30 points after mixing in 70 DEG C of water-baths
Clock is let cool, and is neutralized to neutrality with sodium hydroxide test solution, is diluted to 20ml, as system suitability solution with mobile phase；Precision amount
20 μ l are taken to inject liquid chromatograph；
Measuring method
It takes this product fine powder appropriate, add flowing phased soln and is diluted in every 1ml containing about the solution of phenprobamate 2mg, shake up, filter
It crosses, as test solution；Precision measures in right amount, is quantitatively diluted with mobile phase and solution of every 1ml containing about 20 μ g is made, as right
According to solution；20 μ l test solutions and contrast solution are taken, liquid chromatograph, record spectrogram to main peak retention time are injected separately into
2 times；
<3>dissolution test；
<4>HPLC method assay.
2. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<1>presses following operation
It carries out: taking this product fine powder appropriate, add ethyl alcohol 20ml, grinding dissolution filters, and water bath method takes residue, measures in accordance with the law.
3. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<3>is according to dissolution rate
It is measured with drug release determination method: taking this product, using pH1.2 hydrochloric acid solution 900ml as dissolution medium, revolving speed is 50 turns per minute, according to
Method operation, when through 45 minutes, takes solution to filter in right amount, discards at least 10ml primary filtrate, take subsequent filtrate as test solution；Separately
Precision weighs phenprobamate reference substance 22mg, sets in 100ml measuring bottle, and methanol 5ml is added to make to dissolve, then solubilization goes out medium to quarter
Degree, shakes up, as reference substance solution；It takes above two solution according to UV-VIS spectrophotometry, is surveyed at the wavelength of 260nm
Determine absorbance, calculates every the amount of dissolution.
4. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<4>is according to efficient liquid
Phase chromatography measurement；
Chromatographic condition and system suitability
It is filler with octadecylsilane chemically bonded silica, using methanol-water 50:50 as mobile phase；Detection wavelength is 259nm；Claim
Phenprobamate reference substance about 20mg is taken, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, heats 30 points after mixing in 70 DEG C of water-baths
Clock is let cool, and is neutralized to neutrality with sodium hydroxide test solution, is diluted to 20ml, as system suitability solution with mobile phase；Precision amount
20 μ l are taken to inject liquid chromatograph；
Measuring method
This product 20 are taken, accurately weighed, finely ground, precision measurement fine powder is appropriate, is placed in 100ml volumetric flask, and it is suitable that mobile phase is added
Amount dissolution, and it is diluted to scale, it shakes up, filters, take subsequent filtrate as test solution；Reference substance about 10mg is separately taken, precision claims
It is fixed, flowing phased soln is added and quantifies the solution that the 0.4mg containing phenprobamate in every 1ml is made in dilution；Precision measures above-mentioned solution
Each 20 μ l, is injected separately into liquid chromatograph, according to external standard method with calculated by peak area.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015534A (en) * | 2005-09-26 | 2007-08-15 | 刘凤鸣 | Sustained release preparation of phenprobamate |
| WO2015072853A1 (en) * | 2013-11-13 | 2015-05-21 | Rjg Developments B.V. | Treatment of herpes virus infection outbreaks |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2891459B1 (en) * | 2005-09-30 | 2007-12-28 | Flamel Technologies Sa | MICROPARTICLES WITH MODIFIED RELEASE OF AT LEAST ONE ACTIVE INGREDIENT AND ORAL GALENIC FORM COMPRISING THE SAME |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015534A (en) * | 2005-09-26 | 2007-08-15 | 刘凤鸣 | Sustained release preparation of phenprobamate |
| WO2015072853A1 (en) * | 2013-11-13 | 2015-05-21 | Rjg Developments B.V. | Treatment of herpes virus infection outbreaks |
Non-Patent Citations (3)
| Title |
|---|
| The rapid quantitative analysis of phenprobamate and acetaminophen by RP-LC and compensation technique;M. Levent Altun等;《Journal of Pharmaceutical and Biomedical Analysis》;20011231;第25卷;第85-92页 * |
| 反相高效液相色谱法测定苯丙氨酯片的含量;余小平等;《医药导报》;20050831;第24卷(第8期);第720页第2节 * |
| 紫外分光光度法测定苯丙氨酯片含量的研究;田勇;《天津药学》;19990831;第11卷(第3期);第51页第3节 * |
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