CN112630252A - Nondestructive testing method for stability of tablet containing antioxidant butyl hydroxy anisole - Google Patents

Nondestructive testing method for stability of tablet containing antioxidant butyl hydroxy anisole Download PDF

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CN112630252A
CN112630252A CN202011224200.7A CN202011224200A CN112630252A CN 112630252 A CN112630252 A CN 112630252A CN 202011224200 A CN202011224200 A CN 202011224200A CN 112630252 A CN112630252 A CN 112630252A
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tablet
sample
stability
epr
antioxidant
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CN112630252B (en
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王欣雨
周新波
裘雅渔
胡秀荣
俞卡茜
方伟杰
高建青
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Zhejiang University ZJU
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/10Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using electron paramagnetic resonance

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Abstract

The invention discloses a nondestructive testing method for the stability of a tablet containing an antioxidant butylated hydroxyanisole, which comprises the following steps of (1) putting a tablet forming sample whole tablet containing the antioxidant butylated hydroxyanisole into an EPR sample tube and weighing the sample whole tablet; (2) putting an EPR sample tube filled with the tablet finished medicine into an EPR resonant cavity, and ensuring that the sample is positioned in the center of the resonant cavity; (3) detecting the tablet after tuning; (4) and (4) performing secondary integration on the obtained spectrogram, correcting the obtained secondary integration area by adopting the sample quality to obtain a sample stability parameter, and judging according to the sample stability parameter. The invention applies the EPR technology to the stability detection of the tablet finished medicine containing the antioxidant butyl hydroxy anisole for the first time, and expands the application range of the EPR technology; the method has simple steps, realizes the nondestructive and efficient detection of the stability of the tablet finished product containing the antioxidant butyl hydroxy anisole, and has high sensitivity.

Description

Nondestructive testing method for stability of tablet containing antioxidant butyl hydroxy anisole
Technical Field
The invention relates to the technical field of drug stability detection, in particular to a nondestructive testing method for the stability of a tablet containing an antioxidant butylated hydroxyanisole.
Background
The development of drugs faces many technical challenges, especially for structurally unstable drugs, induced degradation by light, moisture, heat, etc. easily occurs. The stability of the drug may not only affect the efficacy of the drug, but also may create safety issues. Factors that affect drug stability include the structure of the drug itself, interactions between drug molecules, and its physical form. The process optimization of bulk drugs and pharmaceutical preparations to maintain the stability thereof is the key to the successful development of drugs. Therefore, a great deal of manpower, financial resources and material resources are invested in drug research and development institutions to study the stability of drug raw materials and preparations in the production and storage processes.
The existing common analysis method for the stability of the medicine is a chromatographic method such as high performance liquid chromatography, but chromatographic conditions have great influence on detection results, for example, the medicine is oxidized to lose an H atom and become a free radical, the site for removing the H atom is not single, the direct separation and analysis of the H atom are quite difficult, each medicine needs to search different solvent ratios and detection parameters, a series of work such as making a quantitative standard curve and the like, so that the difficulty of separating and identifying the stability of the medicine by adopting the chromatographic method is large, the time consumption is long, the expansion is difficult, and how to simply, conveniently and rapidly judge the stability of the medicine is still a difficult problem at present. In addition, the conventional chromatography requires a series of operations such as grinding and dissolving of a drug sample, which may cause secondary degradation of the sample. Therefore, a novel nondestructive and efficient drug stability research method is developed, and the method has a practical value.
Electron paramagnetic resonance spectroscopy (EPR) is the only technology capable of directly detecting free radical signals, and information on the states, contents and other aspects of free radicals can be obtained through research on EPR spectral lines, so that the EPR technology has wide application in the fields of physics, chemistry and the like. However, free radicals generated by drug degradation are very active and difficult to detect by using EPR, so that no relevant report of applying the EPR technology to drug stability research is found so far.
Disclosure of Invention
The invention aims to provide a nondestructive testing method for stability of a tablet containing antioxidant butylated hydroxyanisole, which applies an EPR (ethylene-propylene-rubber) detection technology to the stability detection of finished tablets containing antioxidant butylated hydroxyanisole and has the advantages of simple steps, high detection sensitivity, rapid quantitative detection, nondestructive detection and the like.
In order to achieve the purpose, the invention adopts the following technical scheme: the nondestructive testing method for the stability of the tablet containing the antioxidant butyl hydroxy anisole comprises the following steps:
(1) the tablet-forming sample monolith containing the antioxidant butylated hydroxyanisole was placed in an EPR sample tube and weighed, with the weight in m and units in g. At present, when the stability of the tablet finished medicine is detected, the tablet finished medicine is ground into powder, the sample is easy to degrade and deteriorate due to the grinding of the powder, the detection result is influenced, and the grinding wastes time; free radicals generated by drug degradation are very active and are difficult to detect by using EPR, so that no relevant report about the application of the EPR technology in drug stability determination exists; the inventor of the invention finds out by accident that the stability of the tablet patent medicine containing the antioxidant butylated hydroxyanisole can be rapidly, quantitatively and nondestructively detected by utilizing an EPR technology, the tablet patent medicine can be directly detected without grinding and crushing, and the detection efficiency is greatly improved; the reason for this is probably that the antioxidant butylated hydroxyanisole can provide available hydrogen ions for radical acceptance to form stable radicals, and thus can be detected by EPR (the stability of antioxidant butylated hydroxyanisole is judged by detecting the more stable radicals after reaction with the deteriorated radicals by EPR).
(2) And (3) putting the EPR sample tube filled with the tablet finished medicine into an EPR resonant cavity, and ensuring that the sample is positioned in the center of the resonant cavity.
(3) After tuning, the tablet is detected, and the detection parameters are set as follows: the detection power is 2-20 mW, and the central magnetic field is 2000-4000G, the field width of 400-4000G, the microwave frequency modulation of 100kHz, the microwave amplitude modulation of 1-2G, the time constant of 40.96-163.84 msec, the conversion time of 20-80 msec, the number of scanning points of 1000-4000 and the gain of 102~105The number of scanning times is 1-20.
(4) And (3) performing secondary integration on the obtained spectrogram, recording the area of the secondary integration as s, recording the detection power as p, recording the gain as r, recording the scanning times as n and the sample mass as m, and correcting the obtained area of the secondary integration by adopting the sample mass to obtain a sample stability parameter, wherein the calculation formula is as follows: sample stability parameter = s/(n × p × r × m × 10)4). The lower the sample stability parameter, the better the tablet formulation stability of the tablet containing the antioxidant butylated hydroxyanisole; the higher the sample stability parameter, the poorer the stability of the tablet formulation containing the antioxidant butylated hydroxyanisole.
Preferably, in the step (1), the tablet drug forming sample containing the antioxidant butylated hydroxyanisole is simvastatin tablet, lovastatin tablet or enzalutamide tablet.
Preferably, in the step (1), the EPR sample tube is a round-bottom tube or a flat-bottom tube made of quartz, and the diameter of the EPR sample tube is 10 mm. The EPR sample tube is made of quartz, so that extra background signals cannot be brought, and the detection result is not influenced; the diameter is 10mm, and the tablet can be put down to form a medicine and can be put into an EPR resonant cavity.
Preferably, in step (1), the stacking height of the tablet finished medicine sample in the EPR sample tube is 5 +/-0.2 cm. The stacking height of the tablet finished medicine sample in the EPR sample tube is 5 +/-0.2 cm, so that the samples are distributed at all heights of the EPR resonant cavity, the absorption efficiency is consistent, and the detection result is more accurate; too high or too low, the absorbed energy of the sample is inconsistent, and the accuracy of the result obtained by detection is extremely low.
Preferably, in step (3), the detection power is 20 mW. The conventional EPR detection power is 2mW, the signal intensity can be enhanced by improving the test power, but signals with overhigh power are easy to saturate, 20mW is better power after trial, the higher the amplitude modulation is in the EPR test, the stronger the signals are, but the poorer the resolution is, because the stability parameters of the sample are only required to be qualitatively detected and determined, the amplitude modulation can be properly improved, and meanwhile, the scanning time constant is prolonged and the signals are superposed, so that the effects of improving the test sensitivity and the signal intensity are achieved, the content of free radical impurities in a medicine sample is extremely low, and a clear spectrogram easy to analyze can be obtained.
Preferably, in step (3), the central magnetic field is 3000G, and the scanning field width is 2000G.
Preferably, in step (3), the microwave amplitude is 2G.
Preferably, in step (3), the time constant is 80.96msec, the switching time is 40msec, the number of scanning points is 2000, and the number of scanning times is 16.
Therefore, the invention has the following beneficial effects: the EPR technology is applied to the stability detection of the tablet finished medicine containing the antioxidant butyl hydroxy anisole for the first time, and the application range of the EPR technology is expanded; as long as weigh after the fixed dress appearance height, can calculate the stability parameter that obtains the sample according to the secondary integral area of sample quality and EPR spectrogram, can judge the stability that the tablet that contains antioxidant butyl hydroxy anisole becomes the medicine through stability parameter size, the step is simple, has realized the harmless, high-efficient detection to the tablet that contains antioxidant butyl hydroxy anisole becomes medicine stability, and sensitivity is high.
Drawings
FIG. 1 is an EPR detection spectrum in comparative example 1.
FIG. 2 is an EPR detection spectrum in comparative example 2.
FIG. 3 is an EPR detection spectrum in example 1.
FIG. 4 is an EPR detection spectrum in comparative example 1.
FIG. 5 is an EPR detection spectrum in example 2.
FIG. 6 is an EPR detection spectrum in example 3.
FIG. 7 is an EPR detection spectrum in example 4.
FIG. 8 is an EPR detection spectrum in example 5.
FIG. 9 is an EPR detection spectrum in example 6.
FIG. 10 is an EPR detection spectrum in example 7.
FIG. 11 is an EPR detection spectrum in example 8.
FIG. 12 is an EPR detection spectrum in example 9.
Detailed Description
The invention is further described with reference to the following figures and detailed description. The commercially available pharmaceuticals of the following examples of the invention all contain the antioxidant BHA (which can be retrieved by the FDA).
Comparative example 1
(1) Adopting a self-made simvastatin tablet (without adding any antioxidant), and adopting a formula (in parts by weight, 150 parts of simvastatin, 2 parts of ascorbic acid, 2 parts of citric acid, 30 parts of hydroxypropyl cellulose, 10 parts of hydroxypropyl methylcellulose, 5 parts of ferric oxide, 200 parts of lactose, 5 parts of magnesium stearate, 400 parts of microcrystalline cellulose, 200 parts of starch, 5 parts of talcum powder and 3 parts of titanium dioxide), blowing and heating at 50 ℃ for 5 hours, putting the whole tablet into an EPR sample tube, weighing the tablet, wherein the EPR sample tube is a flat-bottom tube made of quartz, and the diameter of the EPR sample tube is 10 mm; the stack height of the simvastatin tablet sample in the EPR sample tube is 4.8cm, and the weight is weighed to be 3.2 g.
(2) And (3) putting the EPR sample tube filled with the tablet finished medicine into an EPR resonant cavity, and ensuring that the sample is positioned in the center of the resonant cavity.
(3) After tuning, the tablet is detected, and the detection parameters are set as follows: the detection power is 20mW, the central magnetic field is 3000G, the scanning field width is 2000G, the microwave frequency modulation is 100kHz, the microwave amplitude modulation is 2G, the time constant is 80.96msec, the conversion time is 40msec, the number of scanning points is 2000, and the gain is 2 multiplied by 104The scanning times are 16 times; the obtained spectrum is shown in FIG. 1.
As can be seen from FIG. 1, the detected free radical signal intensity is weak (the signal-to-noise ratio is low, the line is very uneven), which indicates that the simvastatin metamorphic product is difficult to directly detect by using EPR.
Comparative example 2
Comparative example 2 was compared with comparative example 1 except that 0.1 part of butylhydroxyanisole as an antioxidant was added to the formulation, the weight was 3.2g, and the sample was heated by blowing at 50 ℃ for 5 hours and then packed in an EPR sample tube, which was otherwise identical with comparative example 1. The obtained spectrum is shown in FIG. 2.
As can be seen from FIG. 2, there is a clear free radical signal generated in the spectrum, which indicates that the deterioration degree of simvastatin can be detected by the EPR technique after adding butylated hydroxyanisole.
Example 1
Example 1 was different from comparative example 1 in that a commercially available simvastatin tablet (brand: ZOCOR; manufacturer: Merck & Co., Inc., specification 0.2 g/tablet, date of production 2019, 12 months) was selected, the stacking height was 4.8cm, the weight was 3.2g, and the rest was identical to comparative example 1. The obtained spectrum is shown in FIG. 3.
As can be seen from FIG. 3, the spectrum is a background signal, and almost no free radical signal exists, indicating that the stability is better.
Comparative example 1
Comparative example 1 was compared with example 1 except that commercially available simvastatin tablets were pulverized and loaded into EPR sample tubes, and the rest was identical with example 1. The obtained spectrum is shown in FIG. 4.
As can be seen from FIG. 4, there is a very significant generation of free radical signals, indicating that the grinding affects the detection results of simvastatin tablets.
Example 2
This example is different from example 1 in that the date of manufacture of simvastatin tablets was 16 years and 7 months, and the gain was 2X 103Otherwise, the same procedure as in example 1 was repeated. The obtained spectrum is shown in FIG. 5.
The obtained spectrogram is subjected to secondary integration, and the secondary integration area is (1.52 multiplied by 10)12) And correcting the obtained quadratic integration area by adopting the sample mass, and calculating to obtain a sample stability parameter of 74.22.
Example 3
This example is identical to example 1 except that the date of manufacture of the simvastatin tablet is 18 years and 12 months. The obtained spectrum is shown in FIG. 6.
Integrating the obtained spectrogram twiceThe second integral area is (4.64 multiplied by 10)11) And correcting the obtained secondary integral area by adopting the sample quality, and calculating to obtain a sample stability parameter of 2.27.
Example 4
This example is different from comparative example 1 in that an enzalutamide sheet (brand: xtani; manufacturer: Astellas Pharma inc., specification 0.25 g/sheet) having a production date of 18 years and 12 months was used, the stacking height was 5.2cm, the weight was 0.33g, and the rest was identical to example 1. The obtained spectrum is shown in FIG. 7.
The obtained spectrum was integrated twice, and the area of the second integration was (6.67X 10)12) And correcting the obtained secondary integral area by adopting the sample mass, and calculating to obtain a sample stability parameter of 31.58.
Example 5
This example is identical to example 3 except that the Enzalutamide tablets having a production date of 17 years and 9 months are used and the weight is 0.33 g. The obtained spectrum is shown in FIG. 8.
The obtained spectrogram is subjected to secondary integration, and the secondary integration area is (8.78 multiplied by 10)12) And correcting the obtained quadratic integration area by adopting the sample mass, and calculating to obtain a sample stability parameter of 41.57.
Example 6
This example is identical to example 3 except that the Enzalutamide tablets having a production date of 17 years and 3 months are used and the weight is 0.33g, as compared with example 4. The obtained spectrum is shown in FIG. 9.
The obtained spectrogram is subjected to secondary integration, and the secondary integration area is (1.232 multiplied by 10)13) And correcting the obtained secondary integral area by adopting the sample mass, and calculating to obtain a sample stability parameter of 58.33.
Example 7
(1) Putting commercially available lovastatin tablets (brand: MEVACOR; manufacturer: Merck & Co., Inc., specification of 0.2 g/tablet, production date of 2019 and 8 months) into an EPR sample tube in a whole piece, weighing, wherein the EPR sample tube is a flat-bottom tube made of quartz, and the diameter of the EPR sample tube is 10 mm; the stacking height of the lovastatin tablet sample in the EPR sample tube is 5.1cm, and the weight is weighed to be 3.4 g.
(2) And (3) putting the EPR sample tube filled with the tablet finished medicine into an EPR resonant cavity, and ensuring that the sample is positioned in the center of the resonant cavity.
(3) After tuning, the tablet is detected, and the detection parameters are set as follows: the detection power is 20mW, the central magnetic field is 3000G, the scanning field width is 4000G, the microwave frequency modulation is 100kHz, the microwave amplitude modulation is 2G, the time constant is 81.92msec, the conversion time is 40msec, the number of scanning points is 2000, and the gain is 2 multiplied by 104The scanning times are 16 times; the obtained spectrum is shown in FIG. 10.
The obtained spectrogram is subjected to secondary integration, and the secondary integration area is 1.69 multiplied by 1010And correcting the obtained secondary integral area by adopting the sample quality, and calculating to obtain a sample stability parameter of 0.08.
Example 8
This example is identical to example 7 except that a lovastatin tablet was used in a production date of 2018 and 8 months. The obtained spectrum is shown in FIG. 11.
The obtained spectrogram is subjected to secondary integration, and the secondary integration area is 9.86 multiplied by 1010And correcting the obtained secondary integral area by adopting the sample quality, and calculating to obtain a sample stability parameter of 0.45.
Example 9
This example is identical to example 7 except that a lovastatin tablet was used in a production date of 2018 and 3 months. The obtained spectrum is shown in FIG. 12.
The obtained spectrogram is subjected to secondary integration, and the secondary integration area is 2.81 multiplied by 1011And correcting the obtained secondary integral area by adopting the sample quality, and calculating to obtain a sample stability parameter of 1.29.
As can be seen from fig. 3, 5 and 6, the more early the production date of the simvastatin tablet, the larger the sample stability parameter, and the later the production date of the simvastatin tablet, the smaller the sample stability parameter, and similarly, as can be seen from fig. 7 to 9 and fig. 10 to 12, the earlier the production date of the enzalutamide tablet and the lovastatin tablet, the larger the sample stability parameter, and the later the production date of the enzalutamide tablet and the lovastatin tablet, the smaller the sample stability parameter. Therefore, the invention can carry out nondestructive and efficient detection on the stability of the tablet finished product containing the antioxidant butylated hydroxyanisole, and has high sensitivity.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.

Claims (8)

1. The nondestructive testing method for the stability of the tablet containing the antioxidant butyl hydroxy anisole is characterized by comprising the following steps:
(1) putting the tablet-shaped whole medicine sample containing the antioxidant butylated hydroxyanisole into an EPR sample tube, weighing, recording the weight as m, and measuring the unit as g;
(2) putting an EPR sample tube filled with the tablet finished medicine into an EPR resonant cavity, and ensuring that the sample is positioned in the center of the resonant cavity;
(3) after tuning, the tablet is detected, and the detection parameters are set as follows: the detection power is 2-20 mW, the central magnetic field is 2000-4000G, the field sweeping width is 400-4000G, the microwave frequency modulation is 100kHz, the microwave amplitude modulation is 1-2G, the time constant is 40.96-163.84 msec, the conversion time is 20-80 msec, the number of scanning points is 1000-4000, and the gain is 102~105Scanning for 1-20 times;
(4) and (3) carrying out secondary integration on the obtained spectrogram, recording the area of the secondary integration as s, recording the detection power as p, recording the gain as r, recording the scanning frequency as n, and correcting the obtained area of the secondary integration by adopting the sample quality to obtain a sample stability parameter, wherein the calculation formula is as follows: sample stability parameter = s/(n × p × r × m × 10)4)。
2. The method for nondestructive testing of the stability of the tablet containing the antioxidant butylated hydroxyanisole as claimed in claim 1, wherein in the step (1), the tablet drug forming sample containing the antioxidant butylated hydroxyanisole is simvastatin tablet, lovastatin tablet or enzalutamide tablet.
3. The nondestructive testing method for the stability of the tablet containing the antioxidant butylated hydroxyanisole as claimed in claim 1, wherein in step (1), the EPR sample tube is a round-bottom tube or a flat-bottom tube made of quartz, and the diameter of the EPR sample tube is 10 mm.
4. The nondestructive testing method for the stability of the tablet containing the antioxidant butylated hydroxyanisole as claimed in claim 1, wherein in the step (1), the stacking height of the tablet finished product sample in the EPR sample tube is 5 ± 0.2 cm.
5. The method for the nondestructive examination of the stability of the tablet containing the antioxidant butylated hydroxyanisole as claimed in claim 1, wherein in the step (3), the detection power is 20 mW.
6. The method for nondestructive testing of tablet stability containing butylated hydroxyanisole as claimed in claim 1, wherein in step (3), the central magnetic field is 3000G and the width of the scanning field is 2000G.
7. The method for nondestructive testing of tablet stability containing butylated hydroxyanisole as an antioxidant as claimed in claim 1, wherein in step (3), microwave amplitude modulation is 2G.
8. The method for nondestructive testing of tablet stability containing butylated hydroxyanisole as an antioxidant of claim 1, wherein in step (3), the time constant is 80.96msec, the switching time is 40msec, the number of scanning points is 2000, and the number of scanning times is 16.
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