CN102095703A - Method for carrying out near infrared spectrum non-destructive analysis on amoxicillin capsules - Google Patents
Method for carrying out near infrared spectrum non-destructive analysis on amoxicillin capsules Download PDFInfo
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- CN102095703A CN102095703A CN 201010601369 CN201010601369A CN102095703A CN 102095703 A CN102095703 A CN 102095703A CN 201010601369 CN201010601369 CN 201010601369 CN 201010601369 A CN201010601369 A CN 201010601369A CN 102095703 A CN102095703 A CN 102095703A
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Abstract
The invention relates to a method for carrying out near infrared spectrum non-destructive analysis on amoxicillin capsules. The method is characterized by comprising the following steps of: 1) selecting amoxicillin capsules of n batches, wherein the content of amoxicillin is 83.281-85.353%, and determining the average value of the amoxicillin content of each batch; 2) selecting at least six amoxicillin capsules of each batch, and acquiring a near infrared diffuse reflection spectrum by a diffuse reflection optical-fiber probe; 3) preprocessing the near infrared diffuse reflection spectrum to obtain a second derivative spectrum; 4) carrying out data association on the average value of the amoxicillin content obtained in the step 1) and the second derivative spectrum obtained in the step 3) to obtain a mathematical model of the amoxicillin content; and 5) acquiring the near infrared diffuse reflection spectrum of the amoxicillin capsules the amoxicillin content of which is required to be determined, and substituting the near infrared diffusion reflection spectrum into the mathematical model obtained in the step 4), thus the amoxicillin content is obtained. By applying the method provided by the invention, capsule coating and aluminium foil package are not required to be removed, the analysis is rapid, simple and convenient, and the result is accurate.
Description
Technical field
The invention belongs to the pharmaceutical preparation analysis technical field, particularly a kind of near infrared spectrum nondestructive analysis method of Biomox.
Background technology
The Amoxicillin content assaying method of stipulating in the pharmacopeia is a high performance liquid chromatography, concrete experimental technique is as follows: get the content under the content uniformity item, mix, precision is measured (being equivalent to Amoxicillin 0.125g approximately), add the moving phase dissolving and be diluted to the solution that contains 0.5mg among every 1ml approximately, filter, get subsequent filtrate, precision is measured 20 μ l and is injected liquid chromatograph, the record chromatogram; It is an amount of that other gets the Amoxicillin reference substance, measures with method.Go out C in the test sample by external standard method with calculated by peak area
16H
19N
3O
5The content of S.Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filling agent; (regulating pH value to 5.0 with the 2mol/L potassium hydroxide solution)-acetonitrile (97.5: 2.5) is a moving phase with the 0.05mol/L potassium dihydrogen phosphate; Flow velocity is the about 1ml of per minute; The detection wavelength is 254nm.Number of theoretical plate calculates by the Amoxicillin and is not less than 2000.
Above-mentioned analytical approach relates to weighing, dissolving, filtration, the record of chromatogram and a large amount of Chemical Pretreatment steps such as configuration of damping fluid of Biomox, operate loaded down with trivial details relatively, the particularly preparation of phosphate buffer and demarcation, consuming time longer, bring many inconvenience to real work.
Near-infrared spectrum analysis is that spectral measurement methods, the stoichiometry of infrared range (800-2500nm) nearly learns a skill, computer technology and basic test technology are intersected the modern analytical technique that combines, and is mainly used in the direct express-analysis of complex sample.The maximum characteristics of this analytical approach are that sample is not had invasive with destructive; Simple to operate, analyze rapidly, once analyzing only needs tens seconds to a few minutes; The instrument low price, use cost is low; Measuring-signal can long-distance transmissions and analysis; Particularly combine with computer technology and optical fiber technology, adopt optical detecting methods such as NIR transmission, scattering, diffuse reflection, can not use chemical reagent, do not carry out sample pretreatment, directly graininess, solid shape, pasty state, opaque and transparent sample such as liquid are analyzed, therefore, compare with classic method, near infrared spectrum is used for the pharmaceutical preparation analysis and has unique advantage.
People such as the Shen Yi of Shanghai Drug Control Inst. have delivered the research paper of " near-infrared diffuse reflectance spectrometry is to the qualitative and quantitative test of amoxil capsule ", the result shows with near-infrared spectral analysis technology amoxil capsule is carried out the qualitative and quantitative analysis result accurately and reliably, method is easy fast, do not need pre-service, can be applied to the original position and the online detection of this type of sample industry spot.Place the near infrared sample cup to detect sample powder art after needing in this research paper implementation process amoxil capsule taken apart.
Summary of the invention
The purpose of this invention is to provide a kind of can overcome above-mentioned defective, simple to operate, analyze near infrared spectrum nondestructive analysis method rapid, nondestructive Biomox.Its technical scheme is:
A kind of near infrared spectrum nondestructive analysis method of Biomox is characterized in that adopting following steps:
1) chooses n batch the amoxil capsule of Amoxicillin content between 83.281～85.353%, according to the method requirement in 2005 editions second one of the Pharmacopoeia of the People's Republic of China, measure the mean value of Amoxicillin content in each batch amoxil capsule, wherein n is not less than 40;
2) each batch chosen m grain amoxil capsule, and wherein m is not less than 6, pops one's head in diffuse reflection optical fiber and pushes down the acquisition surface near-infrared diffuse reflection spectrum of the amoxil capsule in the step 1), obtains n * m and opens near-infrared diffuse reflection spectrum;
3) with step 2) n * m of obtaining opens near-infrared diffuse reflection spectrum and carries out the spectrum pre-service and obtain n * m and open second derivative spectra;
4) mean value of the Amoxicillin content that step 1) is obtained by chemometrics method and the second derivative spectra that step 3) obtains carry out data association, and the quantitative test spectrum range is 5912.68～4859.74cm
-1, obtain the mathematical model of Amoxicillin content;
5) according to step 2), gather the near-infrared diffuse reflection spectrum of content amoxil capsule to be measured, and with the mathematical model of this near-infrared diffuse reflection spectrum substitution step 4) gained, promptly get Amoxicillin content, if the Amoxicillin content that obtains is between 83.281～85.353%, then the result is effective, otherwise invalid.
The near infrared spectrum nondestructive analysis method of described Biomox, step 2) to gather in the near-infrared diffuse reflection spectrum, wave-number range is 4000～10000cm
-1, scanning times is not less than 64 times, and resolution is 8cm
-1
The near infrared spectrum nondestructive analysis method of described Biomox, preprocessing procedures adopts the level and smooth and second derivative processing of Norris Derivative filtering in the step 3).
The near infrared spectrum nondestructive analysis method of described Biomox, chemometrics method in the step 4) adopts partial least square method, the second derivative spectra that the indication step 3) obtains is that n * m opens second derivative spectra, and perhaps n * m opens the equal spectrum of n Zhang Ping of second derivative spectra.
The present invention compared with prior art has the following advantages:
Need not Biomox is carried out the pre-treatments such as configuration of the record and the damping fluid of weighing, dissolving, filtration, chromatogram when 1, measuring, environmental protection;
2, simple to operate, analyze rapidly;
3, need not to remove capsule clothing and outermost In Aluminium Foil Packing, can realize the Non-Destructive Testing of sample non-destructive.
Embodiment
Embodiment 1:
1) selects 40 batches commercially available Biomox of Amoxicillin content between 83.281～85.275%, according to the method requirement in 2005 editions second one of the Pharmacopoeia of the People's Republic of China, measure the mean value of Amoxicillin content in each batch amoxil capsule, specifically see Table 1.
The mean value of the Amoxicillin content that table 1 is 40 batches
2) randomly draw 6 Biomoxs from every batch of sample that step 1) obtains, pop one's head in diffuse reflection optical fiber and push down the acquisition surface near-infrared diffuse reflection spectrum of Biomox, wave-number range is 4000～10000cm
-1, scanning times 64 times, resolution is 8cm
-1, obtain the near-infrared diffuse reflection spectrum of every Biomox.
3) adopting the level and smooth and second derivative processing of Norris Derivative filtering to step 2) 240 near-infrared diffuse reflection spectrums of gained carry out the spectrum pre-service, obtain 240 second derivative spectras.
4) select 5912.68～4859.74cm
-1Be the quantitative test spectrum range, the mean value of the Amoxicillin content that step 1) is obtained by partial least square method and 240 second derivative spectras that step 3) obtains carry out data association, set up the mathematical model of Amoxicillin content.
5) according to step 2), select 10 batches of amoxil capsules that content is to be measured, randomly draw 1 amoxil capsule in every batch of sample and carry out the near-infrared diffuse reflection spectrum collection, and with the mathematical model of this near-infrared diffuse reflection spectrum substitution step 4) gained, promptly get Amoxicillin content, specifically see Table 2.
The actual content data record according to step 1) in the table 2, and the prediction content data records according to step 5), and the relative error data are ((prediction content data-actual content data)/actual content data) * 100.Analysis result shows that the relative error of method has good content prediction ability between-0.458～0.125%, can satisfy Amoxicillin analysis on Content requirement.
The actual content of the Amoxicillin that table 2 is 10 batches and the contrast of prediction content
| Sample number | Actual content (%) | Prediction content (%) | Relative error (%) |
| 1 | 85.172 | 85.058 | -0.134 |
| 2 | 84.670 | 84.282 | -0.458 |
| 3 | 84.397 | 84.373 | -0.028 |
| 4 | 84.219 | 84.036 | -0.217 |
| 5 | 84.500 | 84.563 | 0.075 |
| 6 | 84.969 | 84.753 | -0.254 |
| 7 | 84.453 | 84.481 | 0.033 |
| 8 | 84.497 | 84.603 | 0.125 |
| 9 | 84.851 | 84.906 | 0.065 |
| 10 | 85.123 | 85.134 | 0.013 |
Embodiment 2:
1) selects 48 batches commercially available Biomox of Amoxicillin content between 83.312～85.353%, according to the method requirement in 2005 editions second one of the Pharmacopoeia of the People's Republic of China, measure the mean value of Amoxicillin content in each batch amoxil capsule, specifically see Table 3.
The mean value of the Amoxicillin content that table 3 is 48 batches
2) randomly draw 6 Biomoxs from every batch of sample that step 1) obtains, pop one's head in diffuse reflection optical fiber and push down the acquisition surface near-infrared diffuse reflection spectrum of Biomox, wave-number range is 4000～10000cm
-1, scanning times 64 times, resolution is 8cm
-1, obtain the near-infrared diffuse reflection spectrum of every Biomox.
3) adopting the level and smooth and second derivative processing of Norris Derivative filtering to step 2) 288 near-infrared diffuse reflection spectrums of gained carry out the spectrum pre-service, obtain 288 second derivative spectras.
4) select 5912.68～4859.74cm
-1Be the quantitative test spectrum range, the mean value of the Amoxicillin content that step 1) is obtained by partial least square method and 288 second derivative spectras that step 3) obtains carry out data association, set up the mathematical model of Amoxicillin content.
5) according to step 2), select 13 batches of amoxil capsules that content is to be measured, randomly draw 1 amoxil capsule in every batch of sample and carry out the near-infrared diffuse reflection spectrum collection, and with the mathematical model of this near-infrared diffuse reflection spectrum substitution step 4) gained, promptly get Amoxicillin content, specifically see Table 4.
The actual content data record according to step 1) in the table 4, and the prediction content data records according to step 5), and the relative error data are ((prediction content data-actual content data)/actual content data) * 100.Analysis result shows that the relative error of method has good content prediction ability between-0.295～0.467%, can satisfy Amoxicillin analysis on Content requirement.
The actual content of the Amoxicillin that table 4 is 13 batches and the contrast of prediction content
| Sample number | Actual content (%) | Prediction content (%) | Relative error (%) |
| 1 | 84.738 | 84.734 | -0.005 |
| 2 | 84.507 | 84.855 | 0.412 |
| 3 | 84.514 | 84.613 | 0.117 |
| 4 | 84.321 | 84.499 | 0.211 |
| 5 | 83.942 | 84.334 | 0.467 |
| 6 | 84.577 | 84.736 | 0.188 |
| 7 | 84.172 | 84.436 | 0.314 |
| 8 | 84.554 | 84.752 | 0.234 |
| 9 | 84.818 | 84.700 | -0.139 |
| 10 | 84.585 | 84.448 | -0.162 |
| 11 | 84.754 | 84.504 | -0.295 |
| 12 | 84.253 | 84.362 | 0.129 |
| 13 | 84.479 | 84.257 | -0.263 |
Embodiment 3:
Step is identical with embodiment 1, and just: the second derivative spectra that the indication step 3) obtains in the step 4) is the equal spectrum of 40 Zhang Pings of 240 second derivative spectras.10 batches Amoxicillin content data according to the present embodiment gained specifically sees Table 5.
The actual content of the Amoxicillin that table 5 is 10 batches and the contrast of prediction content
| Sample number | Actual content (%) | Prediction content (%) | Relative error (%) |
| 1 | 85.172 | 85.066 | -0.124 |
| 2 | 84.670 | 84.283 | -0.457 |
| 3 | 84.397 | 84.373 | -0.028 |
| 4 | 84.219 | 84.037 | -0.216 |
| 5 | 84.500 | 84.553 | 0.063 |
| 6 | 84.969 | 84.735 | -0.275 |
| 7 | 84.453 | 84.418 | -0.041 |
| 8 | 84.497 | 84.630 | 0.157 |
| 9 | 84.851 | 84.690 | -0.190 |
| 10 | 85.123 | 85.077 | -0.054 |
The actual content data record according to step 1) in the table 5, and the prediction content data records according to step 5), and the relative error data are ((prediction content data-actual content data)/actual content data) * 100.Analysis result shows that the prediction relative standard deviation of method has good content prediction ability between-0.457～0.157%, can satisfy Amoxicillin analysis on Content requirement.
Claims (6)
1. the near infrared spectrum nondestructive analysis method of a Biomox is characterized in that adopting following steps:
1) chooses n batch the amoxil capsule of Amoxicillin content between 83.281～85.353%, according to the method requirement in 2005 editions second one of the Pharmacopoeia of the People's Republic of China, measure the mean value of Amoxicillin content in each batch amoxil capsule, wherein n is not less than 40;
2) each batch chosen m grain amoxil capsule, and wherein m is not less than 6, pops one's head in diffuse reflection optical fiber and pushes down the acquisition surface near-infrared diffuse reflection spectrum of the amoxil capsule in the step 1), obtains n * m and opens near-infrared diffuse reflection spectrum;
3) with step 2) n * m of obtaining opens near-infrared diffuse reflection spectrum and carries out the spectrum pre-service and obtain n * m and open second derivative spectra;
4) mean value of the Amoxicillin content that step 1) is obtained by chemometrics method and the second derivative spectra that step 3) obtains carry out data association, and the quantitative test spectrum range is 5912.68～4859.74cm
-1, obtain the mathematical model of Amoxicillin content;
5) according to step 2), gather the near-infrared diffuse reflection spectrum of content amoxil capsule to be measured, and with the mathematical model of this near-infrared diffuse reflection spectrum substitution step 4) gained, promptly get Amoxicillin content, if the Amoxicillin content that obtains is between 83.281～85.353%, then the result is effective, otherwise invalid.
2. the near infrared spectrum nondestructive analysis method of Biomox as claimed in claim 1 is characterized in that: step 2) to gather in the near-infrared diffuse reflection spectrum, wave-number range is 4000～10000cm
-1, scanning times is not less than 64 times, and resolution is 8cm
-1
3. the near infrared spectrum nondestructive analysis method of Biomox as claimed in claim 1 is characterized in that: the level and smooth and second derivative processing of preprocessing procedures employing Norris Derivative filtering in the step 3).
4. the near infrared spectrum nondestructive analysis method of Biomox as claimed in claim 1 is characterized in that: the chemometrics method employing partial least square method in the step 4).
5. the near infrared spectrum nondestructive analysis method of Biomox as claimed in claim 1, it is characterized in that: the second derivative spectra that the indication step 3) obtains in the step 4) is that n * m opens second derivative spectra.
6. the near infrared spectrum nondestructive analysis method of Biomox as claimed in claim 1, it is characterized in that: the second derivative spectra that the indication step 3) obtains in the step 4) is the equal spectrum of n Zhang Ping that n * m opens second derivative spectra.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539373A (en) * | 2011-12-21 | 2012-07-04 | 无锡济民可信山禾药业股份有限公司 | Method for quick and nondestructive measurement of aldioxa content in aldioxa raw material and preparation |
| CN112263569A (en) * | 2020-11-05 | 2021-01-26 | 南京致中生物科技有限公司 | Amoxicillin capsule and preparation method thereof |
| CN113522152A (en) * | 2021-09-17 | 2021-10-22 | 江西鼎峰智能装备有限公司 | Powder mixing system, control method and powder intensified mixing method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999059554A1 (en) * | 1998-05-15 | 1999-11-25 | Nasa/Johnson Space Center | In situ activation of microcapsules |
| CN101776675A (en) * | 2008-08-27 | 2010-07-14 | 广州联创思远利生物科技有限公司 | Novel detection method of injection use compound amoxicillin sodium and clavulanate potassium |
-
2010
- 2010-12-23 CN CN 201010601369 patent/CN102095703A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999059554A1 (en) * | 1998-05-15 | 1999-11-25 | Nasa/Johnson Space Center | In situ activation of microcapsules |
| CN101776675A (en) * | 2008-08-27 | 2010-07-14 | 广州联创思远利生物科技有限公司 | Novel detection method of injection use compound amoxicillin sodium and clavulanate potassium |
Non-Patent Citations (3)
| Title |
|---|
| 《中国抗生素杂志》 20020630 程存归 等 漫反射傅里叶变换红外光谱定量分析方法 全文 1-6 第27卷, 第6期 2 * |
| 《安徽医药》 20100831 朱健永 等 维生素B2片快速检验的近红外漫反射光谱法定量模型初探 第902-904页 1-6 第14卷, 第8期 2 * |
| 《药物分析杂志》 20050430 沈漪 等 近红外漫反射光谱法对阿莫西林胶囊的定性及定量分析 第385-386页 1-6 第25卷, 第4期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539373A (en) * | 2011-12-21 | 2012-07-04 | 无锡济民可信山禾药业股份有限公司 | Method for quick and nondestructive measurement of aldioxa content in aldioxa raw material and preparation |
| CN102539373B (en) * | 2011-12-21 | 2014-08-06 | 无锡济民可信山禾药业股份有限公司 | Method for quick and nondestructive measurement of aldioxa content in aldioxa raw material and preparation |
| CN112263569A (en) * | 2020-11-05 | 2021-01-26 | 南京致中生物科技有限公司 | Amoxicillin capsule and preparation method thereof |
| CN112263569B (en) * | 2020-11-05 | 2022-07-08 | 贝克诺顿(浙江)制药有限公司 | Amoxicillin capsule and preparation method thereof |
| CN113522152A (en) * | 2021-09-17 | 2021-10-22 | 江西鼎峰智能装备有限公司 | Powder mixing system, control method and powder intensified mixing method |
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Application publication date: 20110615 |