CN111103368B - Method for predicting validity period of esomeprazole enteric-coated tablet - Google Patents
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Abstract
The invention relates to the technical field of prediction of drug expiration date, and particularly discloses a method for predicting the expiration date of esomeprazole enteric-coated tablets, wherein the method takes the impurity content with the relative retention time of 0.35 in a high-performance liquid chromatogram of the esomeprazole enteric-coated tablets obtained by a related substance detection method in 2015-edition pharmacopoeia as an index, analyzes the index content in different temperature and humidity environments to obtain a curve of the impurity content changing along with time and an expiration date T under corresponding temperature T and humidity RH conditions, performs linear regression on 1/T and RH by ln1/T, and predicts the shelf life of the esomeprazole enteric-coated tablets under specific storage temperature and humidity by using an Arrhenius equation corrected by humidity. The validity period prediction equation established by the invention has the advantages of short test period, good repeatability and reliable prediction result.
Description
Technical Field
The invention relates to the technical field of prediction of drug validity period, in particular to a method for predicting the validity period of esomeprazole enteric-coated tablets.
Background
Esomeprazole is a proton pump inhibitor, can specifically act on parietal cells of gastric mucosa, irreversibly inhibits the activity of H +/K + -ATP enzyme in the parietal cells, has strong and lasting gastric acid inhibition effect, and can effectively treat gastroesophageal reflux disease. The esomeprazole enteric-coated tablet has high bioavailability and is an outstanding medicament for treating peptic ulcer. However, the preparation process of the product is complex, the problem of stability is easy to occur in the imitation process, if a stability test method specified by pharmacopoeia is adopted, the time is long, the cost is high, manpower and material resources are consumed, in order to shorten the time and improve the efficiency, an effective period prediction model needs to be established, the degradation rule of the medicine is found out, and the effective period is presumed.
The existing method for predicting the validity period of esomeprazole enteric-coated tablets comprises methods such as software prediction, a classical constant temperature method, a multi-element linear model method, an initial average speed method and an Arrhenius equation prediction method for humidity correction, wherein the method comprises the steps of quantifying the influence degree of environmental factors on chemical reaction by using chemical kinetics, selecting indexes which are the content of active ingredients, placing products under severe conditions for accelerating destruction to accelerate the deterioration of the products, sampling at certain time intervals, analyzing the indexes, detecting the validity period under the conditions, and establishing a prediction formula by using fitting curves of the validity period and temperature or humidity under different temperatures and humidity, so that prediction is carried out, but the accuracy and repeatability of the predicted result are poor, and the result is unreliable.
Disclosure of Invention
Aiming at the problems of low accuracy, poor repeatability and unreliable prediction result of the existing method for predicting the valid period of esomeprazole enteric-coated tablets, the invention provides a method for predicting the valid period of the esomeprazole enteric-coated tablets.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a method for predicting the effective period of esomeprazole enteric-coated tablets comprises the steps of carrying out high performance liquid chromatography detection on the esomeprazole enteric-coated tablets by using a method for detecting related substances in 2015 pharmacopoeia, taking the content of impurities with retention time of 0.35 relative to the chromatographic peak of esomeprazole in a chromatogram as an index, respectively placing the esomeprazole enteric-coated tablets in different temperature and humidity environments, sampling for a plurality of times according to preset sampling time to analyze the index content, obtaining a curve of the impurity content changing along with the time under the corresponding temperature T and humidity RH conditions, calculating the time T when the mass content of the impurity is increased to 0.2 percent, performing linear regression on 1/T and RH by ln1/T, according to the humidity-corrected Arrhenius equation, an equation for predicting the shelf life of esomeprazole enteric-coated tablets is established, and the shelf life of the esomeprazole enteric-coated tablets under specific storage temperature and humidity is predicted by using the equation.
Wherein, when the mass content of the impurities is increased to 0.2 percent, the effective components of the esomeprazole enteric-coated tablet are reduced, and the drug effect is lost.
Compared with the prior art, the method for predicting the effective period of the esomeprazole enteric-coated tablets provided by the invention has the advantages that the impurity content with the relative retention time of 0.35 in a high-performance liquid chromatogram of the esomeprazole enteric-coated tablets obtained by a related substance detection method in the 2015-edition pharmacopoeia is used as an index, the deterioration of the esomeprazole enteric-coated tablets is accelerated by setting temperature and humidity conditions, a curve of the change of the impurity index content along with time under the accelerated deterioration condition is obtained, an equation for predicting the effective period of the esomeprazole enteric-coated tablets is quickly established by an Arrhenius equation for humidity correction, the effective period of the esomeprazole enteric-coated tablets under the normal storage environment condition is deduced, the theoretical derivation is simple, the test period is short, the repeatability is good, the prediction result is consistent with the actual effective period of a medicine, and the accuracy is high.
The detection conditions of the high performance liquid chromatography in the detection method of the related substances in the 2015-edition pharmacopoeia of the esomeprazole enteric-coated tablet are as follows:
a chromatographic column: octadecylsilane chemically bonded silica gel column;
mobile phase: the mobile phase A is water-phosphate buffer solution-acetonitrile with the volume ratio of 80:10: 10; the mobile phase A is acetonitrile-phosphate buffer solution-water with the volume ratio of 80:1:19, and the pH value of the phosphate buffer solution is 7.6; wherein, each 1000ml of phosphate buffer solution contains 0.0052mol of sodium dihydrogen phosphate and 0.0315mol of disodium hydrogen phosphate;
Column temperature: at 37 ℃;
detection wavelength: 302 nm;
sample introduction volume: 20 mu L of the solution;
elution conditions: 0-10min, 100-80 vol% of phase A and 0-20 vol% of phase B; 10-30min, 80-0 vol% of phase A and 20-100 vol% of phase B; 30-31min, 0-100 vol% of phase A and 100-0 vol% of phase B; 31-45min, 100 vol% of phase A and 0 vol% of phase B;
the preparation method of the test solution comprises the following steps: precisely weighing 20mg of esomeprazole, placing the esomeprazole into a 100ml measuring flask, adding 10ml of methanol, shaking, adding 20ml of phosphate buffer solution (0.0137 mol of sodium phosphate and 0.0551mol of disodium hydrogen phosphate in each 1000 ml) with pH of 11.0, shaking, dissolving the esomeprazole by ultrasound, diluting the solution to a scale with water, filtering, and taking the filtrate as a test solution.
Preferably, the established equation for predicting the effective period of the esomeprazole enteric-coated tablet is ln1/T ═ 16824.43/T +0.013RH +45.26, wherein T is the effective period and has the unit of h; t is the temperature in Kelvin, in K; RH is humidity in%.
Preferably, the temperature setting range in the environment with different temperature and humidity is 50-65 ℃, and the humidity setting range is 29-75%.
Preferably, 5-6 different temperature and humidity environments are set in the temperature and humidity range.
Preferably, the temperature environment is provided by an electrothermal forced air drying oven.
Preferably, the humidity environment is provided by a saturated salt solution of the corresponding humidity.
Preferably, the time required for detecting the impurity content to increase by 0.02-0.03% in the corresponding temperature and humidity environment through a pre-experiment is used as the interval sampling time to obtain the preset sampling time.
Preferably, the time required for detecting each increase of the impurity content by 0.02% in the corresponding temperature and humidity environment through a pre-experiment is used as the interval sampling time, so as to obtain the preset sampling time.
The temperature and humidity environment and the sampling time points are specifically selected and shown in the following table:
drawings
Fig. 1 is a high performance liquid chromatogram of esomeprazole enteric-coated tablets in an example of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Detecting the content of impurities in the esomeprazole enteric-coated tablet by using a high performance liquid chromatography method for detecting related substances in 2015 pharmacopoeia, wherein the specific detection conditions are as follows:
a chromatographic column: agilent Eclipse XDB C18, 4.6X 150mm, 3.5 μm;
Mobile phase: the mobile phase A is water-phosphate buffer solution-acetonitrile with the volume ratio of 80:10: 10; the mobile phase A is acetonitrile-phosphate buffer solution-water with the volume ratio of 80:1:19, and the pH value of the phosphate buffer solution is 7.6; wherein, each 1000ml of phosphate buffer solution contains 0.0052mol of sodium dihydrogen phosphate and 0.0315mol of disodium hydrogen phosphate;
column temperature: 37 ℃;
detection wavelength: 302 nm;
sample introduction volume: 20 mu L of the solution;
elution conditions: 0-10min, 100-80 vol% of phase A and 0-20 vol% of phase B; 10-30min, 80-0 vol% of phase A and 20-100 vol% of phase B; 30-31min, 0-100 vol% of phase A and 100-0 vol% of phase B; 31-45min, 100 vol% of phase A and 0 vol% of phase B;
precisely weighing 20mg of esomeprazole enteric-coated tablet, placing the tablet in a 100ml measuring flask, adding 10ml of methanol, shaking, adding 20ml of phosphate buffer solution (the content of sodium phosphate is 0.0137mol/L, the content of disodium hydrogen phosphate is 0.0551mol/L, pH is 11.0), shaking, ultrasonically dissolving esomeprazole, diluting with water to scale, filtering, and taking the filtrate as a sample solution.
The obtained chromatogram is shown in figure 1, the retention time of the peak 1 relative to esomeprazole (peak 2) is 0.35, the impurities are used as indexes, esomeprazole enteric-coated tablets are respectively placed in the temperature and humidity environments shown in table 1, the time required for detecting that the impurity content increases by 0.02% in the corresponding temperature and humidity environments through pre-experiments is used as interval sampling time to obtain the preset sampling time points shown in table 1, the esomeprazole enteric-coated tablets are respectively placed in the 6 temperature and humidity environments shown in table 1, six tablets are placed in each temperature and humidity environment and are ground into fine powder, sampling is carried out according to the sampling time points in table 1, the amount of one tablet of medicinal powder is taken in each sampling, the index impurity content of a sampling sample is detected, curves of the index impurity content changing along with time in the 6 temperature and humidity environments are obtained, the time T when the mass content of the index impurities under the corresponding temperature T and humidity RH conditions reaches 0.2% is calculated, namely the limited period of the esomeprazole enteric-coated tablet under the temperature T and humidity RH conditions, according to an Arrhenius equation ln 1/T-Ea/RT + BRH + lnA corrected by humidity, linear regression is carried out on 1/T and RH by ln1/T, and the established effective period prediction equation is ln 1/T-16824.43/T +0.013RH +45.26, wherein T is the effective period and the unit is h; t is the temperature in Kelvin, in K; RH is humidity in%.
TABLE 1 six temperature and humidity environments and sampling time
Wherein, the temperature and humidity environment with T65/DEG C and RH 75% is that the esomeprazole enteric-coated tablet is fixed above the saturated sodium chloride solution, then the sodium chloride solution and the esomeprazole enteric-coated tablet are put into an electric heating forced air drying oven for constant temperature and humidity accelerated test;
the temperature and humidity environment with the temperature T being 60/DEG C and the RH being 50% is that the esomeprazole enteric-coated tablet is fixed above a saturated sodium bromide solution, then the sodium bromide solution and the esomeprazole enteric-coated tablet are placed into an electrothermal blowing dry box, and a constant temperature and humidity accelerated test is carried out;
the temperature and humidity environment with the temperature T being 60/DEG C and the RH being 29% is that the esomeprazole enteric-coated tablet is fixed above a saturated magnesium chloride solution, and then the magnesium chloride solution and the esomeprazole enteric-coated tablet are placed into an electrothermal blowing drying oven for constant temperature and humidity accelerated test;
the temperature and humidity environment with the temperature T being 55/DEG C and the RH being 50% is that the esomeprazole enteric-coated tablet is fixed above a saturated sodium bromide solution, then the sodium bromide solution and the esomeprazole enteric-coated tablet are placed into an electrothermal blowing dry box, and a constant temperature and humidity accelerated test is carried out;
the temperature and humidity environment with the temperature of 50/DEG C and the RH of 29 percent is that the esomeprazole enteric-coated tablet is fixed above a saturated magnesium chloride solution, and then the magnesium chloride solution and the esomeprazole enteric-coated tablet are put into an electrothermal blowing dry box for a constant temperature and humidity accelerated test.
Example 2
The shelf life prediction equation ln 1/T-16824.43/T +0.013RH +45.26 of the esomeprazole enteric-coated tablet with the conventional storage temperature T of 30 ℃ (303K) and the packaging humidity RH of 5% was substituted into the shelf life prediction equation ln 1/T-16824.43/T +0.013RH +45.26 in example 1, and the shelf life was calculated to be 36.06 months.
Three batches of esomeprazole enteric-coated tablets (P1, P2 and P3) are respectively placed in an environment with the temperature of 30 ℃ and the humidity of 5% for long-term storage and continuous sampling detection, when the impurity content with the relative retention time of 0.35 in P1 reaches 0.197%, the storage time is 36 months, when the impurity content with the relative retention time of 0.35 in P2 reaches 0.2%, the storage time is 36 months, and when the impurity content with the relative retention time of 0.35 in P3 reaches 0.196%, the storage time is 36 months.
Example 3
When T ═ 30 ℃ (303K) and RH ═ 20% were put into the expiration date prediction equation ln1/T ═ 16824.43/T +0.013RH +45.26 in example 1, the expiration date of esomeprazole enteric-coated tablets under the temperature and humidity storage conditions was predicted to be 29.67 months.
The three batches of esomeprazole enteric-coated tablets (P1, P2 and P3) in example 2 were placed in respective environments with a temperature of 35 ℃ and a storage humidity of 20% respectively for long-term storage and continuous sampling detection, and the storage time was 30 months when the impurity content with a relative retention time of 0.35 in P1 reached 0.199%, 29.5 months when the impurity content with a relative retention time of 0.35 in P2 reached 0.195%, and 29.5 months when the impurity content with a relative retention time of 0.35 in P2 reached 0.197%.
Example 4
When T35 ℃ (308K) and RH 5% are put into the expiration date prediction equation ln 1/T-16824.43/T +0.013RH +45.26 in example 1, the expiration date of esomeprazole enteric-coated tablets under the temperature and humidity storage conditions is predicted to be 14.66 months.
The three batches of esomeprazole enteric-coated tablets (P1, P2 and P3) in example 2 were placed in respective environments with a temperature of 35 ℃ and a storage humidity of 5% respectively for long-term storage and continuous sampling detection, and the storage time was 15 months when the impurity content with a relative retention time of 0.35 in P1 reached 0.199%, 15 months when the impurity content with a relative retention time of 0.35 in P2 reached 0.21%, and 15 months when the impurity content with a relative retention time of 0.35 in P3 reached 0.199%.
The effective period of the esomeprazole enteric-coated tablet obtained by the prediction method in the embodiment 2-4 is consistent with the effective period time detected by actual storage, the accuracy is high, the repeatability is good, and a rapid and reliable method is provided for predicting the effective period of the esomeprazole enteric-coated tablet.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the invention is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (6)
1. A method for predicting the validity period of esomeprazole enteric-coated tablets is characterized by comprising the following steps: performing high performance liquid chromatography detection on esomeprazole enteric-coated tablets by using a method for detecting related substances in 2015 pharmacopoeia, taking the content of impurities in a chromatogram which is 0.35 relative to the chromatographic peak retention time of the esomeprazole as an index, respectively placing the esomeprazole enteric-coated tablets in different temperature and humidity environments, performing sampling analysis on the index content for a plurality of times according to preset sampling time to obtain a curve of the content of the impurities along with time change under corresponding temperature T and humidity RH conditions, calculating the time T when the mass content of the impurities is increased to 0.2%, performing linear regression on 1/T and RH by using ln1/T, establishing an equation for predicting the effective period of the esomeprazole enteric-coated tablets according to an Arrhenius equation for humidity correction, and predicting the shelf life of the esomeprazole enteric-coated tablets under a specific storage temperature and humidity by using the equation.
2. The method for predicting the expiration date of esomeprazole enteric tablet of claim 1, wherein: the established equation for predicting the effective period of the esomeprazole enteric-coated tablet is ln 1/T-16824.43/T +0.013RH +45.26, wherein T is the effective period and the unit is h; t is the temperature in Kelvin, in units of K; RH is humidity in%.
3. The method for predicting the expiration date of esomeprazole enteric tablet of claim 1, wherein: the temperature setting range in the different temperature and humidity environments is 50-65 ℃, and the humidity setting range is 29-75%.
4. The method for predicting the shelf life of esomeprazole enteric tablet of claim 3, wherein: and 5-6 different temperature and humidity environments are set in the temperature and humidity range.
5. The method for predicting the shelf life of esomeprazole enteric tablet of claim 1, wherein: and detecting the time required for increasing the impurity content by 0.02-0.03% in the corresponding temperature and humidity environment through a pre-experiment to be used as the interval sampling time, so as to obtain the preset sampling time.
6. The method for predicting the shelf life of esomeprazole enteric tablet of claim 1, wherein: and detecting the time required for increasing the impurity content by 0.02% in the corresponding temperature and humidity environment through a pre-experiment to be used as interval sampling time, so as to obtain the preset sampling time.
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