CN107543881A - The method of quality control of phenprobamate piece - Google Patents
The method of quality control of phenprobamate piece Download PDFInfo
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- CN107543881A CN107543881A CN201710732845.3A CN201710732845A CN107543881A CN 107543881 A CN107543881 A CN 107543881A CN 201710732845 A CN201710732845 A CN 201710732845A CN 107543881 A CN107543881 A CN 107543881A
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Abstract
The invention discloses a kind of method of quality control of phenprobamate piece, the problem of method exists for the relevant quality of the pharmaceutical preparations detection method of existing phenprobamate piece is improved, it is main to be the increase in IR discriminatings, Related substances separation, dissolution test, and assay is carried out using HPLC methods.The present invention method of quality control it is reasonable in design, accurately and reliably, specificity it is strong and simple 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, ensure that production technology is controllable, ensure Clinical practice safety, reliable guarantee is definitely provided for product curative effect is stable.
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 technology
Phenprobamate (Phenprobamate) be it is a kind of have contrastimulant central skeletal muscle relaxant, earliest by
Siegfried successfully synthesizes in nineteen sixty, is listed first in Japan and Germany.Tianjin Zhongxin Pharmaceutical Group Co., Ltd. in
The certification for obtaining raw material first in 1981；The same year, Tianjin Lisheng Pharmaceutical Co., Ltd. obtain the certification of tablet.This product is in state
A kind of interior only formulation 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 inflammation, rheumatic arthritis, ligament injury, myotenositis around shoulder neck joint, additionally for youngster
The auxiliary treatment of virgin Lennox-Gastaut syndromes.
The standard of phenprobamate tablet only exists《Chinese Pharmacopoeia》Nineteen ninety-five version two was recorded, 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.The document of relevant phenprobamate raw material and tablet to deliver is fewer, at present
The document relevant with quality standard mainly has：(1)《The content of rp-hplc determination phenprobamate piece》Yu little Ping,
Zhang Zhi's root；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 about key indexs such as material, 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.Therefore, existing method is difficult to effectively control production
In final product quality, the quality of different batches of product can not ensure product curative effect without rationally accurately index is weighed,
Clinical treatment is influenceed huge.
The content of the invention
The technical problem to be solved in the present invention is to provide it is a kind of it is reasonable in design, accurately and reliably, specificity it is strong and simple to operate
Phenprobamate piece method of quality control, to help the final product quality in effectively control phenprobamate piece production and improve its matter
Amount is horizontal, it is ensured that Clinical practice curative effect.
In order to solve the above technical problems, the present invention uses following technical scheme：
The method of quality control of phenprobamate piece, comprises the following steps：
<1>IR differentiates；
<2>Related substances separation；
<3>Dissolution test；
<4>HPLC method assays.
Step<1>Carried out by following operation：Take this product fine powder appropriate, add ethanol 20ml, grinding dissolving, filtration, water-bath steaming
It is dry, residue is taken, is determined in accordance with the law.
Step<2>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；Weigh phenprobamate reference substance about 20mg, add mobile phase 5ml to dissolve, add hydrochloric acid 1ml, mix after in 70 DEG C of water-baths plus
Heat 30 minutes, lets cool, neutrality is neutralized to sodium hydroxide test solution, 20ml, as system suitability solution are diluted to mobile phase；
Precision measures 20 μ l injection liquid chromatographs；
Determination method
Take this product fine powder appropriate, add flowing phased soln and be diluted in every 1ml containing about phenprobamate 2mg solution, shake up,
Filtration, as need testing 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 need testing solutions and contrast solution are taken, is injected separately into liquid chromatograph, record spectrogram to main peak retention time
2 times.
Step<3>Determined according to dissolution rate and drug release determination method：This product is taken, using pH1.2 hydrochloric acid solutions 900ml as dissolution
Medium, rotating speed are 50 turns per minute, are operated in accordance with the law, during through 45 minutes, take solution to filter in right amount, discard at least 10ml primary filtrates,
Subsequent filtrate is taken as need testing solution；Another precision weighs phenprobamate reference substance 22mg, puts in 100ml measuring bottles, adds methanol 5ml to make
Dissolving, then solubilization go out medium to scale, shake up, as reference substance solution；Above two solution is taken to shine UV-vis spectroscopy
Photometry, absorbance is determined at 260nm wavelength, calculates every stripping quantity.
Step<4>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；Weigh phenprobamate reference substance about 20mg, add mobile phase 5ml to dissolve, add hydrochloric acid 1ml, mix after in 70 DEG C of water-baths plus
Heat 30 minutes, lets cool, neutrality is neutralized to sodium hydroxide test solution, 20ml, as system suitability solution are diluted to mobile phase；
Precision measures 20 μ l injection liquid chromatographs；
Determination method
This product 20 is taken, accurately weighed, finely ground, it is appropriate that precision measures fine powder, is placed in 100ml volumetric flasks, adds flowing
Mutually appropriate dissolving, and scale is diluted to, shake up, filter, take subsequent filtrate as need testing solution；Reference substance about 10mg separately is taken, essence
It is close weighed, add flowing phased soln and quantify 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, are injected separately into liquid chromatograph, according to external standard method with calculated by peak area.
The problem of existing for the relevant quality of the pharmaceutical preparations detection method of existing phenprobamate piece, inventor is improved, main
IR discriminatings, Related substances separation, dissolution test are the increase in, and assay is carried out using HPLC methods.The present invention's
Method of quality control is reasonable in design, accurately and reliably, specificity it is strong and simple to operate, establish the new quality control of phenprobamate piece accordingly
Standard processed, it 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, ensure that production technology is controllable, it is ensured that Clinical practice safety, reliable guarantee is definitely provided for product curative effect is stable.
Brief description of the drawings
Fig. 1 is phenprobamate control collection of illustrative plates (Chinese Pharmacopoeia infrared spectrum collection Figure 22 9).
Fig. 2 is phenprobamate reference substance infrared spectrogram.
Fig. 3 is phenprobamate piece infrared spectrogram.
Fig. 4 is the relevant material chromatogram of phenprobamate.
Fig. 5 is the stripping curve of each factory's phenprobamate piece.
Fig. 6 is the stripping curve of the multiple batches of phenprobamate piece of B factories.
Fig. 7 is the stripping curve of the multiple batches of phenprobamate piece of C factories.
Fig. 8 is the system suitability collection of illustrative plates of phenprobamate HPLC assays.
Fig. 9 is phenprobamate raw material typical case's collection of illustrative plates.
Figure 10 is phenprobamate piece need testing solution typical case's collection of illustrative plates.
Figure 11 is three kinds of method assay results contrast figures.
Embodiment
The method of quality control research of phenprobamate piece
Through inquiring about national general bureau's database, phenprobamate only has a kind of formulation of tablet, 1 specification, is 200mg.This grinds
Study carefully and extracted multiple producers totally 96 batch phenprobamate piece.
<1>IR differentiates
By using technological means such as powder x-ray diffraction, infrared spectrum, near infrared spectrums, phenprobamate is compareed
Product, raw material and raw material recrystallised sample are analyzed, and do not find that three's collection of illustrative plates has differences, thus prove phenprobamate raw material
It should be single crystal form.
After being recrystallized due to phenprobamate ethanol, chloroform and water, IR collection of illustrative plates and reference substance collection of illustrative plates, collection of illustrative plates holding one is compareed
Cause, therefore tablet can extract measure IR spectrum after phenprobamate with ethanol, establish the IR Hyperspectral indexes of tablet.The benzene drafted
Third urethane piece infrared spectrum discrimination method is as follows：
Take this product fine powder appropriate (being approximately equivalent to phenprobamate 200mg), add ethanol 20ml, grinding dissolving, filtration, water-bath steaming
It is dry, residue is taken, is determined in accordance with the law；The infrared absorption pattern of this product should be with the collection of illustrative plates (figure of Chinese Pharmacopoeia infrared spectrum collection 229) that compares
Unanimously.
Method detects each batch phenprobamate piece, gained IR collection of illustrative plates (Fig. 3, each batch result are similar) and reference substance figure like this
Spectrum is (see Fig. 2), control collection of illustrative plates is consistent (see Fig. 1).
<2>Related substances separation
With reference to documents and materials and experimental exploring, attempt to establish relevant material in phenprobamate raw material and tablet using HPLC methods
The method of inspection.Method has carried out mobile phase investigation, the selection of Detection wavelength, solvent is selected, specificity is investigated, linear relationship is examined
Examine, the methods of stability of solution, sample introduction precision, test limit and limit determine learns research work, the Related substances separation drafted
Method is as follows：
Determined 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；Weigh phenprobamate reference substance about 20mg, add mobile phase 5ml to dissolve, add hydrochloric acid 1ml, mix after in 70 DEG C of water-baths plus
Heat 30 minutes, lets cool, neutrality is neutralized to sodium hydroxide test solution, 20ml, as system suitability solution are diluted to mobile phase；
Precision measures 20 μ l injection liquid chromatographs；The separating degree of phenylpropanol (relative retention time is about 0.9) and phenprobamate should accord with
Close and require；
Determination method
Take this product fine powder appropriate, add flowing phased soln and be diluted in every 1ml containing about phenprobamate 2mg solution, shake up,
Filtration, as need testing 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 need testing solutions and contrast solution are taken, is injected separately into liquid chromatograph, record spectrogram to main peak retention time
2 times；If any impurity peaks in need testing solution, single impurity peak area cannot be greater than 0.3 times of contrast solution main peak area
(0.3%), each impurity peak area and cannot be 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 successively impurity 1~6 is named as by retention time.The content that each impurity detects in raw material and tablet
Scope 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 the phenprobamate of table 1 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 below 0.5%, and the quality of product is preferable.Because of partial supplementary material peak and impurity peaks separating degree
Less, during consideration routine check, all auxiliary materials are calculated by impurity peaks, the single miscellaneous content of maximum of tablet is 0.29%, always miscellaneous to contain
Measure as 0.84%.According to the studies above result, with reference to domestic production technological level, formulating limit of impurities level is：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 solutions, pH4.0 acetate delay
Fliud flushing and pH6.8 phosphate buffers) in dissolution rate have larger difference, dissolution rate is maximum in pH1.2 hydrochloric acid solutions, therefore
It is determined that using pH1.2 hydrochloric acid solutions as the dissolution medium of phenprobamate piece.Using water 900ml as dissolution medium, in 50 revs/min of rotating speed
Under conditions of, when most domestic producer sample was through 45 minutes, stripping quantity exceedes the 75% of labelled amount, with reference to Japanese orange peel
Book, it is 50 revs/min to determine dissolution test rotating speed, and sample time is 45 minutes.The phenprobamate piece dissolution test drafted
It is as follows：
Determined according to dissolution rate and drug release determination method (method of Chinese Pharmacopoeia general rule 0,931 second)：This product is taken, with pH1.2 salt
Acid solution 900ml is dissolution medium, and rotating speed is 50 turns per minute, is operated in accordance with the law, during through 45 minutes, takes solution to filter in right amount, abandons
At least 10ml primary filtrates are gone, take subsequent filtrate as need testing solution；Another precision weighs phenprobamate reference substance 22mg, puts 100ml
In measuring bottle, add methanol 5ml dissolving, then solubilization is gone out medium to scale, shake up, as reference substance solution；Take above two
Solution shines UV-VIS spectrophotometry, and absorbance is determined at 260nm wavelength, calculates every stripping quantity, and limit is mark
The 75% of the amount of showing, regulation should be met.
The phenprobamate piece of the phenprobamate piece of method detection different manufacturers and the different batches of same producer like this, institute
Obtain stripping curve such as Fig. 5~7.As shown in figure 5, when most domestic producer sample was through 45 minutes, stripping quantity exceedes labelled amount
75%, and batch between dissolution difference less (Fig. 6, other producers are substantially similar), it is molten but when having the product of one through 45 minutes
The 70% of the below standard amount of showing of output, and batch between dissolution it is widely different (Fig. 7).This prompts the production technology and its stably of the producer
Problem be present in property.
<4>HPLC method assays
With reference to documents and materials and experimental exploring, the HPLC content assaying methods of phenprobamate raw material and tablet, allusion quotation are established
Type chromatogram is shown in Fig. 8~10.The phenprobamate piece HPLC method assays drafted are as follows：
Determined 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；Weigh phenprobamate reference substance about 20mg, add mobile phase 5ml to dissolve, add hydrochloric acid 1ml, mix after in 70 DEG C of water-baths plus
Heat 30 minutes, lets cool, neutrality is neutralized to sodium hydroxide test solution, 20ml, as system suitability solution are diluted to mobile phase；
Precision measures 20 μ l injection liquid chromatographs；The separating degree of phenylpropanol (relative retention time is about 0.9) and phenprobamate should accord with
Close and require；
Determination method
This product 20 is taken, accurately weighed, finely ground, precision measures fine powder in right amount (equivalent to phenprobamate 40mg), is placed in
In 100ml volumetric flasks, add mobile phase and dissolve in right amount, and be diluted to scale, shake up, filter, take subsequent filtrate molten as test sample
Liquid；Another to take reference substance about 10mg, accurately weighed, addition, which flows phased soln and quantifies dilution and be made in every 1ml, contains phenprobamate
0.4mg solution；Precision measures each 20 μ l of above-mentioned 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 (see figure according to the content results of UV methods, nitriding, Syrups by HPLC respectively
11), the HPLC methods measurement result of most of sample is closer to nitriding measurement result, and UV methods are because using old lot number reference substance
Experiment, most of assay are relatively low.Meanwhile influence of the auxiliary material in measure is investigated with blank auxiliary, as a result show：Using fixed
When nitrogen method determines phenprobamate piece content, blank auxiliary is noiseless.
Measured result is analyzed with SPSS16.0 softwares, analysis result shows, 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 methods, UV methods replication 20 times, is examined with t and carries out method ratio
Compared with.As a result show：Significant difference (being shown in Table 2) be present in three kinds of methods.The result of wherein nitriding measure determines than HPLC method
Result it is high by 2.7%, it is higher by 3.5% than UV method measurement results.Wherein UV methods because reference substance problem, measurement result it is relatively low, it is not recommended that
Assay for tablet；The scope of gap mean of access allowable error 2% between HPLC methods and nitriding.
Consider that HPLC methods are slightly better than nitriding from the convenience of assay method.
Therefore, nitriding and HPLC methods can Accurate Determining phenprobamate raw material and tablet contents.UV methods are easily disturbed, and are built
View is not used in the assay of the kind.
2 three kinds of method assay result t of table, which are examined, to be compared
Claims (5)
1. a kind of method of quality control of phenprobamate piece, it is characterised in that comprise the following steps：
<1>IR differentiates；
<2>Related substances separation；
<3>Dissolution test；
<4>HPLC method assays.
2. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<1>By following operation
Carry out：Take this product fine powder appropriate, add ethanol 20ml, grinding dissolving, filtration, water bath method, take residue, determine in accordance with the law.
3. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<2>According to efficient liquid
Phase chromatography determines；
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；Claim
Phenprobamate reference substance about 20mg is taken, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, is mixed after 30 points of heating in 70 DEG C of water-baths
Clock, let cool, neutrality is neutralized to sodium hydroxide test solution, 20ml, as system suitability solution are diluted to mobile phase；Precision amount
20 μ l are taken to inject liquid chromatograph；
Determination method
Take this product fine powder appropriate, add flowing phased soln and be diluted in every 1ml containing about phenprobamate 2mg solution, shake up, filter
Cross, as need testing 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 need testing solutions and contrast solution are taken, is injected separately into liquid chromatograph, record spectrogram to main peak retention time
2 times.
4. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<3>According to dissolution rate
Determined with drug release determination method：This product is taken, using the hydrochloric acid solution 900ml of pH 1.2 as dissolution medium, rotating speed is 50 turns per minute, according to
Method operates, and during through 45 minutes, takes solution to filter in right amount, discards at least 10ml primary filtrates, take subsequent filtrate as need testing solution；Separately
Precision weighs phenprobamate reference substance 22mg, puts in 100ml measuring bottles, adds methanol 5ml dissolving, then solubilization is gone out medium to quarter
Degree, shakes up, as reference substance solution；Take above two solution to shine UV-VIS spectrophotometry, surveyed at 260nm wavelength
Determine absorbance, calculate every stripping quantity.
5. the method for quality control of phenprobamate piece according to claim 1, it is characterised in that step<4>According to efficient liquid
Phase chromatography determines；
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；Claim
Phenprobamate reference substance about 20mg is taken, adds mobile phase 5ml to dissolve, adds hydrochloric acid 1ml, is mixed after 30 points of heating in 70 DEG C of water-baths
Clock, let cool, neutrality is neutralized to sodium hydroxide test solution, 20ml, as system suitability solution are diluted to mobile phase；Precision amount
20 μ l are taken to inject liquid chromatograph；
Determination method
This product 20 is taken, accurately weighed, finely ground, it is appropriate that precision measures fine powder, is placed in 100ml volumetric flasks, adds mobile phase and fits
Amount dissolving, and scale is diluted to, shake up, filter, take subsequent filtrate as need testing solution；Another to take reference substance about 10mg, precision claims
It is fixed, add flowing phased soln and quantify the solution that the 0.4mg containing phenprobamate in every 1ml is made in dilution；Precision measures above-mentioned solution
Each 20 μ l, are injected separately into liquid chromatograph, according to external standard method with calculated by peak area.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015534A (en) * | 2005-09-26 | 2007-08-15 | 刘凤鸣 | Sustained release preparation of phenprobamate |
| US20090220611A1 (en) * | 2005-09-30 | 2009-09-03 | Frederic Dargelas | Microparticles With Modified Release of At Least One Active Principle and Oral Pharmaceutical Form Comprising Same |
| WO2015072853A1 (en) * | 2013-11-13 | 2015-05-21 | Rjg Developments B.V. | Treatment of herpes virus infection outbreaks |
-
2017
- 2017-08-24 CN CN201710732845.3A patent/CN107543881B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015534A (en) * | 2005-09-26 | 2007-08-15 | 刘凤鸣 | Sustained release preparation of phenprobamate |
| US20090220611A1 (en) * | 2005-09-30 | 2009-09-03 | Frederic Dargelas | Microparticles With Modified Release of At Least One Active Principle and Oral Pharmaceutical Form Comprising Same |
| WO2015072853A1 (en) * | 2013-11-13 | 2015-05-21 | Rjg Developments B.V. | Treatment of herpes virus infection outbreaks |
Non-Patent Citations (4)
| Title |
|---|
| M. LEVENT ALTUN等: "The rapid quantitative analysis of phenprobamate and acetaminophen by RP-LC and compensation technique", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 余小平等: "反相高效液相色谱法测定苯丙氨酯片的含量", 《医药导报》 * |
| 卫生部药典委员会: "《卫生部药品标准（二部）第四册》", 31 December 1995 * |
| 田勇: "紫外分光光度法测定苯丙氨酯片含量的研究", 《天津药学》 * |
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