CN106896162B - A kind of HPLC method of impurity in detection meloxicam tablet - Google Patents
A kind of HPLC method of impurity in detection meloxicam tablet Download PDFInfo
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Abstract
The present invention relates to a kind of HPLC method that can check impurity in meloxicam tablet, this method can effectively detect 0.015 μ g/ml to the meloxicam tablet of 2 μ g/ml concentration ranges, and result is accurate, reliable, has very strong practicability and promotional value.
Description
Technical field
The invention belongs to analysis of pharmaceutical dosage forms methods, are specifically related to a kind of HPLC method for detecting impurity in meloxicam tablet,
The measuring method is stable, accuracy is high.
Background technique
Meloxicam is a kind of non-steroid antiinflammatory of enol amides, has stronger selectivity to Transitional cell carcinomas
Inhibiting effect has the pharmacological actions such as antipyretic, analgesia, anti-inflammatory, and smaller to the toxicity of gastrointestinal tract and kidney.It can be used for rheumatoid
Property arthritis and painful osteoarthritis symptomatic treatment, or related with the skeletal muscle inflammation of control and pain.But in U.S. Lip river former times
Other impurities are readily incorporated during Kang Hecheng, such as: 4- hydroxy-2-methyl -2H-1,2- benzothiazine -3- carboxylic acid, ethyl ester -
1,1- dioxide, 2- amino -5- methylthiazol etc., wherein 2- amino -5- methylthiazol belongs to harmful substance, for organism
There is larger toxicity, Long Term Contact can badly damaged health.In addition, the substance decomposition will affect Meloxicam product quality.
In view of pet has repellency to drug, therefore the dedicated corrigent of pet is added in the dedicated prescription of pet, such as:
Powdered beef, chicken meal, chicken liver meal etc..The introducing of these corrigents disturbs the measurement of impurity, therefore existing detection method is difficult
Impurity and Meloxicam are efficiently separated.
It is directed to the method for detection of the meloxicam tablet in relation to substance at present are as follows:
One, the related substance detecting method of version Chinese Pharmacopoeia Meloxicam piece Meloxicam in 2015: this product is taken, alkali is added
Property methanol solution (take 40% methanol solution 100ml, add 0.4mol/L sodium hydroxide solution 6ml, mix) dissolve and dilute and be made
Solution in every 1ml containing about 1mg, as test solution；Precision measures 1ml, sets in 100ml measuring bottle, with above-mentioned alkaline methanol
Solution is diluted to scale, shakes up, as contrast solution.It is tested according to high performance liquid chromatography (general rule 0512).With octadecyl silicon
Alkane bonded silica gel is filler；With methanol -0.1mol/L ammonium acetate solution (1:1) for mobile phase；Detection wavelength is 270nm.Reason
It is calculated by plate number by Meloxicam peak and is not less than 2000.It takes 20 μ l of contrast solution to inject liquid chromatograph, adjusts detection sensitivity,
The peak height for making principal component chromatographic peak is about the 20% of full scale；It is accurate again to measure test solution and each 20 μ l of contrast solution, point
Not Zhu Ru liquid chromatograph, record chromatogram is to 6 times of principal component peak retention time.It is such as shown in the chromatogram of test solution miscellaneous
Mass peak, single impurity peak area are not greater than 0.5 times (0.5%) of contrast solution main peak area, each impurity peak area and not
Obtain the main peak area (1.0%) greater than contrast solution.
Two, Chinese Journal of Pharmaceuticals (date issued: in November, 2003) HPLC measurement side of the Sino-U.S. Lip river former times in relation to substance
Method are as follows: chromatographic condition: octadecyl silane (5um) be filler, Detection wavelength be 350nm and 260nm, 45 DEG C of column temperature,
Flow velocity 1ml/min, sample volume 20ul.Mobile phase A is 0.1% dipotassium hydrogen phosphate solution (adjustment pH6.0), and Mobile phase B is methanol.
Gradient elution: 0~2.5min, A:B=60:40,；2.5~12min is linearly changed to A:B=30 from A:B=60:40 constant speed:
70.Measuring method: the preparation of solution 1: precision weighs 1 about 0.1g, sets in 50ml volumetric flask, adds 0.4%NaOH solution 6ml, micro-
Temperature, ultrasound make to dissolve, and add 40% methanol constant volume, shake up to obtain the final product.The preparation of solution 2: 1ml in accurate draw solution 1 sets 100ml
In volumetric flask, with 40% methanol constant volume, shake up.Precision draw 1ml 40% methanol constant volume to 10ml, shake up to get.Measurement:
Solution 1,2 is taken to be measured at 350nm and 260nm wavelength.The area of any impurity peaks at 350nm wavelength of solution 1,
It is not greater than the half (0.05%) of 1 peak area at 350nm wavelength of solution 2；Solution 2 any impurity peaks of 260nm area,
It is not greater than 1 peak area (0.1%) at 260nm wavelength of solution 2.Percentage composition of each impurity at high response wave length is calculated,
The sum of all impurity is not greater than 0.3%.
Method in detection method one is compared using isocratic elution method and linear gradient elution method and cannot all be eluted impurity
Come；Method in detection method two needs to detect using the liquid chromatograph and general ultraviolet of being furnished with diode array detector
Device is relatively high compared to price.
Summary of the invention
The object of the present invention is to provide one kind can only reach the method for testing goal with a wavelength, and easy to operate
Facilitate accuracy higher, also reduce cost in the use of instrument, uses the high performance liquid chromatograph for being furnished with UV detector
?.2- amino -5- methylthiazol three kinds of detection methods in terms of detection limit and quantitative limit have all different following tables；
| Project | Method one | Method two | The present invention |
| Detection limit | 10ng/ml | 12.5ng/ml | 7.5ng/ml |
| Quantitative limit | 0.05μg/ml | 0.08μg/ml | 0.03μg/ml |
The HPLC method of impurity, is the mobile phase ratio by changing gradient elution in a kind of detection meloxicam tablet
With the proportion of extracting solution, reaches and the main component in preparation is separated one by one and carries out the measurement in relation to substance.
Gradient elution program of the present invention are as follows:
Mobile phase of the present invention are as follows: 0.2% ammonium dibasic phosphate solution (pH7.0) is mobile phase A；Methanol is B；Isopropyl
Alcohol is mobile phase C.
The preparation method of extracting solution used in the present invention are as follows: take 40% methanol solution 100ml, add 0.4mol/L hydroxide
Sodium solution 6ml is mixed.
The present invention its described in meloxicam tablet major impurity ingredient be 2- amino -5- methylthiazol.The present invention is in this way
Come what is realized:
Chromatographic condition and system suitability with octadecylsilane chemically bonded silica be filler (Thermo C18,
4.6mm × 150mm, 5 μm), 40 DEG C of column temperature；Flow velocity is 0.9mL/min；Detection wavelength is 270nm；
Take meloxicam tablet appropriate, it is finely ground, add extracting solution to be diluted to the solution of every 1ml 0.5mg containing Meloxicam, shakes up,
Filtration, as test solution；
The preparation precision of Meloxicam contrast solution measures test solution 1ml into 100ml volumetric flask, fixed with extracting solution
Hold to scale, shakes up, the solution in every 1mL containing 5ug is obtained, as Meloxicam contrast solution；
Precision measures 20 μ L of contrast solution, injects liquid chromatograph, adjusts detection sensitivity, makes the peak of principal component chromatographic peak
Height is about the 20% of full scale；It is accurate again to measure test solution and each 20 μ l of contrast solution, it is injected separately into liquid chromatograph, is remembered
Chromatogram is recorded to 6 times of principal component retention time.As shown miscellaneous peak in the chromatogram of test solution, relative retention time is less than
0.55 peak is ignored, and the chromatographic peak (2- amino -5- methylthiazol) that relative retention time is 0.59, peak area must not be big
In 0.15 times of contrast solution main peak area, other single impurity peak areas must not cross the 1/2 of contrast solution main peak area
(0.5%), the sum of each impurity peak area is not greater than contrast solution main peak area (1.0%).Less than reference substance solution peak area
It ignores at 0.01 times of peak.The beneficial effects of the present invention are:
The present invention only uses a wavelength that can reach the method for testing goal, and accuracy simple to operate is higher,
Cost is also reduced in the use of instrument, uses the high performance liquid chromatograph for being furnished with UV detector.The present invention is durable
The investigation of property:
The present invention is in the C in relation to selecting 150mm long in substance-measuring method18Chromatographic column, the flowing of durability high spot reviews
The mutually influence of difference pH and column temperature to measuring method.
Influence of 1 flowing phase pH value to content assaying method
In order to investigate flowing phase pH value to the influence in relation to substance detecting method, pH6.5,7.0,7.5 3 are prepared respectively
Mobile phase, other conditions are identical, record chromatogram respectively, compare theoretical cam curve, retention time, content, as a result such as the following table 1 institute
Show.
Influence of the 1 mobile phase difference pH of table to 2- amino -5- methylthiazol
It is obtained by table 1, with the increase of flowing phase pH value, the retention time of 2- amino -5- methylthiazol slightly shifts to an earlier date, and three
Theoretical cam curve, separating degree under the conditions of a meet the requirements, it can be seen that in flowing phase pH value within the scope of 6.5-7.5, tower
Plate number, content meet regulation, illustrate mobile phase pH within the scope of 6.5-7.5,2- amino -5- methylthiazol is more stable.
2 column temperatures are to influence of the invention
In order to investigate column temperature variation to influence of the invention, by column oven control column temperature in test, 30 are set
DEG C, 35 DEG C, 40 DEG C, 45 DEG C of four conditions, respectively acquire relevant temperature under sample chromatographic signal, measuring samples be 1mg/ piece beauty
Lip river former times health tablet preparation compares under different temperatures separating degree, theoretical cam curve, separating degree, content in chromatography graph parameter, as a result as follows
Shown in table 2.
Influence of 2 column temperature of table to 2- amino -5- methylthiazol
It can be seen that the raising with column temperature by upper 2 data of table, the reservation of 2- amino -5- methylthiazol is slightly in advance；No
Under synthermal, the number of plates, the separating degree of 2- amino -5- methylthiazol meet regulation；It can be seen that column temperature is to 2- amino-
The influence of 5- methylthiazol is less.
The HLPC map of mobile phase difference pH and column temperature is shown in attached drawing 1- attached drawing 7 respectively.
Detailed description of the invention:
Attached drawing 1 measures durability HPLC map of the column temperature at 30 DEG C using the present invention
Attached drawing 2 measures durability HPLC map of the column temperature at 35 DEG C using the present invention
Attached drawing 3 measures durability HPLC map of the column temperature at 45 DEG C using the present invention
Attached drawing 4 measures durability HPLC map of the column temperature at 40 DEG C and pH7.0 using the present invention
Attached drawing 5, the durability HPLC map that mobile phase pH6.0 is measured using the present invention
Attached drawing 6, the durability HPLC map that mobile phase pH6.5 is measured using the present invention
Attached drawing 7, the durability HPLC map that mobile phase pH7.5 is measured using the present invention
The HPLC map of attached drawing 8:2- amino -5- methylthiazol detection limit
The HPLC map of attached drawing 9:2- amino -5- methylthiazol quantitative limit
HPLC map of the attached drawing 10:2- amino -5- methylthiazol concentration in 0.25ug/mL
HPLC map of the attached drawing 11:2- amino -5- methylthiazol concentration in 0.5ug/mL
HPLC map of the attached drawing 12:2- amino -5- methylthiazol concentration in 1ug/mL
HPLC map of the attached drawing 13:2- amino -5- methylthiazol concentration in 2ug/mL
HPLC map of the attached drawing 14:2- amino -5- methylthiazol concentration in 4ug/mL
Attached drawing 15:2- amino -5- methylthiazol concentration and peak area relational graph
Attached drawing 16: according to the HPLC map for measuring sample in embodiment 1
Specific embodiment
Following embodiment be to illustrate preferred embodiment of the invention, it will be appreciated by those skilled in the art that with
Lower description is not applied to limit the scope of the invention.
A kind of embodiment one: HPLC method that can check impurity in meloxicam tablet
Measuring samples: 1mg/ piece Meloxicam tablet preparation.(prescription is starch, lactose, Tween 80, Meloxicam, chicken gizzard
Powder, lauryl sodium sulfate)
Chromatographic condition and system suitability with octadecylsilane chemically bonded silica be filler (Thermo C18,
4.6mm × 150mm, 5 μm), 40 DEG C of column temperature；With 0.2% ammonium dibasic phosphate solution (pH7.0) for mobile phase A；Methanol is B；It is different
Propanol solution is mobile phase C.Flow velocity is 0.9mL/min；Detection wavelength is 270nm, carries out gradient elution by following procedure:
The preparation precision of measuring method Meloxicam reference substance solution measures test solution 1ml into 100ml volumetric flask, uses
Extracting solution is settled to scale, shakes up, and the solution in every 1mL containing 5ug is obtained, as Meloxicam reference substance solution.
The preparation of test solution takes meloxicam tablet appropriate, finely ground, and extracting solution is added to be diluted to every 1ml containing Meloxicam
The solution of 0.5mg, shakes up, filtration, as test solution.
Precision measures 20 μ L of reference substance solution, injects liquid chromatograph, adjusts detection sensitivity, makes principal component chromatographic peak
Peak height is about the 20% of full scale；It is accurate again to measure test solution and each 20 μ l of contrast solution, it is injected separately into liquid chromatograph,
Chromatogram is recorded to 6 times of principal component retention time.As shown miscellaneous peak in the chromatogram of test solution, relative retention time is less than
0.55 peak is ignored, and the chromatographic peak (2- amino -5- methylthiazol) that relative retention time is 0.59, peak area must not be big
In 0.15 times of contrast solution main peak area, other single impurity peak areas must not cross the 1/2 of contrast solution main peak area
(0.5%), the sum of each impurity peak area is not greater than contrast solution main peak area (1.0%).Less than reference substance solution peak area
It ignores at 0.01 times of peak.(being shown in Table 3 according to one data of HPLC map of the sample of method measurement)
3 meloxicam tablet defects inspecting result of table
Embodiment two: a kind of the detection limit and quantitative limit of the HPLC method that can check impurity in meloxicam tablet
By 2- amino -5- methylthiazol methanol dilution, 2- amino -5- methylthiazol in the case of different dilutions is recorded
Signal-to-noise ratio, until the response of 2- amino -5- methylthiazol is about 10 times of level of noise in test sample, 2- amino -5- first at this time
Quantifying for base thiazole is limited to 15ng/ml.
By above-mentioned solution methanol dilution, the signal-to-noise ratio of 2- amino -5- methylthiazol in the case of different dilutions is recorded, until
The response of 2- amino -5- methylthiazol is about 3 times of level of noise in test sample, the limit of 2- amino -5- methylthiazol detection at this time
For 5ng/mL (detection limit map is shown in attached drawing 8- attached drawing 9).
A kind of embodiment three: linear relationship experiment for the HPLC method that can check impurity in meloxicam tablet
It is 2ug/mL since 2- amino -5- methylthiazol investigates concentration in this detection method, the present embodiment selects
It is respectively 4.0 μ g/ml, 2.0 μ g/ml, 1.0 μ g/ml, 0.5 μ g/ml that concentration, which is made, with extracting solution in 2- amino -5- methylthiazol
With the solution of 0.25 μ g/ml, shake up, it is accurate respectively to measure in 20 μ L reference substance solutions injection liquid chromatograph, chromatogram is recorded,
Using peak area as ordinate, sample concentration is that abscissa carries out linear regression, and obtained linear map is shown in Figure of description respectively
10- attached drawing 14.
4 2- amino -5- methylthiazol concentration of table and peak area
According to the numerical value in above table, the regression equation y=of 2- amino -5- methylthiazol concentration and peak area has been obtained
0.020x+0.016, coefficient R2=0.999.Concentration is within the scope of 0.25-4 μ g/ml, 2- amino -5- methylthiazol and peak
Area is in good linear relationship.
A kind of example IV: repeatability investigation for the HPLC method that can check impurity in meloxicam tablet
2- amino -5- methylthiazol is configured to the stock solution that concentration is 0.75ug/ml with extracting solution；It is accurate to draw 1ml
Into 100ml volumetric flask to get 0.75 μ g/ml solution, as reference substance solution.Precision weighs 1mg standard quantity meloxicam tablet
In 5g to 100ml volumetric flask, from 1ml is drawn in impurity stock solution into product capacity bottle, ultrasound after appropriate extracting solution is added, it is molten
Xie Houyong dilution is settled to scale.By above two solution respectively into 20 μ l, liquid chromatograph is injected, continuous sample introduction 5 times, is recorded
Chromatogram；As a result it see the table below shown in 5.
The investigation of 5 repetitive test of table
The experimental results showed that the RSD of peak area measurement value illustrates this method to this product with suitable less than 1.0% in repeatability
The property used.
A kind of embodiment five: Intermediate precision test for the HPLC method that can check impurity in meloxicam tablet
It is accurate respectively to claim Tianjin Ringpu Bio-technology Co., Ltd.'s pilot scale amino containing 2- -5- methylthiazol preparation.This hair
Bright method carries out the Intermediate precision test of method, by different operation person, using different instruments, in different time, according to related
Method operates under substance-measuring item, the results are shown in Table 6.
The test of 6 meloxicam tablet Intermediate precision of table
It is obtained by upper table, in different personnel, impurity content in same date measurement sample, the result of six measurements are not marked relatively
Quasi- deviation illustrates that this experimental method Intermediate precision meets the requirements less than 2.0%.
Claims (1)
1. a kind of HPLC method of impurity in detection meloxicam tablet, which is characterized in that gradient elution is used, by meloxicam tablet
In impurity separate and be measured one by one with main component；
The gradient elution program are as follows:
The mobile phase A are as follows: pH 7.0, the ammonium dibasic phosphate solution that concentration is 0.2%；Mobile phase B is methanol；Mobile phase C is
Isopropanol；The meloxicam tablet major impurity is 2- amino -5- methylthiazol；
The HPLC method of impurity, specific implementation step are as follows in the detection meloxicam tablet:
Chromatographic condition and system suitability: being filler with octadecylsilane chemically bonded silica, 40 DEG C of column temperature；Flow velocity is
0.9mL/min；Detection wavelength is 270nm；
The preparation of test solution: taking meloxicam tablet appropriate, finely ground, and extracting solution is added to be diluted to every 1mL 0.5mg containing Meloxicam
Solution, shake up, filter, as test solution；
The preparation of contrast solution: precision measures test solution 1mL and sets in 100mL volumetric flask, is settled to scale with extracting solution, shakes
It is even, the solution of the 5 μ g containing Meloxicam in every 1mL is obtained, as contrast solution；
Precision measures 20 μ L of contrast solution, injects liquid chromatograph, adjusts detection sensitivity, makes the peak height of principal component chromatographic peak about
It is the 20% of full scale；It is accurate again to measure test solution and each 20 μ L of contrast solution, it is injected separately into liquid chromatograph, records color
Spectrogram is to 6 times of principal component retention time, and such as aobvious miscellaneous peak in the chromatogram of test solution, relative retention time is less than 0.55
Peak is ignored, and the chromatographic peak that relative retention time is 0.59 is the chromatographic peak of 2- amino -5- methylthiazol, and peak area must not
Greater than 0.15 times of contrast solution main peak area, other single impurity peak areas must not exceed the 1/2 of contrast solution main peak area,
The sum of each impurity peak area is not greater than contrast solution main peak area, and peak of 0.01 times less than contrast solution main peak area is ignored not
Meter.
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| CN101090900A (en) * | 2004-12-18 | 2007-12-19 | 埃吉斯药物工厂 | Process for preparation of high-purity meloxicam and meloxicam potassium salt |
| CN101437500A (en) * | 2006-05-08 | 2009-05-20 | 株式会社太平洋 | Composition for transdermal absorption and formulation comprising a polymeric matrix formed therefrom |
| CN101632640A (en) * | 2009-06-15 | 2010-01-27 | 陶灵刚 | Meloxicam liposome and pharmaceutical composition thereof |
| CN102775401A (en) * | 2012-08-15 | 2012-11-14 | 青岛农业大学 | Synthesis method of meloxicam |
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| CN101090900A (en) * | 2004-12-18 | 2007-12-19 | 埃吉斯药物工厂 | Process for preparation of high-purity meloxicam and meloxicam potassium salt |
| CN101437500A (en) * | 2006-05-08 | 2009-05-20 | 株式会社太平洋 | Composition for transdermal absorption and formulation comprising a polymeric matrix formed therefrom |
| CN101632640A (en) * | 2009-06-15 | 2010-01-27 | 陶灵刚 | Meloxicam liposome and pharmaceutical composition thereof |
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