CN106769953A - A kind of method of the content of magnesium in measure omeprazole magnesium crude medicine - Google Patents
A kind of method of the content of magnesium in measure omeprazole magnesium crude medicine Download PDFInfo
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- CN106769953A CN106769953A CN201710178335.6A CN201710178335A CN106769953A CN 106769953 A CN106769953 A CN 106769953A CN 201710178335 A CN201710178335 A CN 201710178335A CN 106769953 A CN106769953 A CN 106769953A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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Abstract
The content of magnesium in omeprazole magnesium crude medicine is determined the present invention relates to Flame Atomic Absorption Spectrophotometry, by sample pre-treatments, prepare magnesium standard curve, the method Accurate Determining content of magnesium content of content of magnesium is determined using atomic absorption spectrophotometry, optimal Operating parameters are determined, method sensitivity for analysis is high, accuracy is high, it is simple with sample handling processes, reduce the disturbing factor in determining, the advantages of operability is good, can provide accurate data for magnesium omeprazole medicine control process.
Description
Technical field
Present invention relates particularly to a kind of assay method of the content of magnesium in magnesium omeprazole, belong to chemical analysis method neck
Domain.
Background technology
The diseases such as the heartburn and sour regurgitation that magnesium omeprazole clinically causes for hyperhydrochloria.Pharmacopoeia of People's Republic of China two
Portion（2015 editions）Magnesium omeprazole enteric coatel tablets are included, classification is proton pump inhibitor, but the existing 2015 editions Chinese people are total to
Omeprazole magnesium crude medicine is not included with state pharmacopeia.Therefore need to grind omeprazole magnesium crude medicine quality standard
Study carefully, research detection method should meet Pharmacopoeia of People's Republic of China four（2015 editions）Code requirement, it is ensured that produce
Omeprazole magnesium crude medicine quality conformance and reliability.The present invention determines magnesium omeprazole using Flame Atomic Absorption Spectrophotometry
Middle content of magnesium has simultaneously carried out methodological study.Purpose is to overcome method disunity in the prior art, and precision and accuracy are low
Defect.
The content of the invention
It is high it is an object of the invention to provide a kind of precision and accuracy, it is easy to operate, and can be magnesium omeprazole
Medicine control process provides the method for determining content of magnesium in magnesium omeprazole of accurate data.
The described method comprises the following steps：
The treatment of sample：
Need testing solution：It is accurate to weigh the uniform sample 0.2500g of crushing（It is accurate to 0.0001g）It is placed in 50ml beakers, plus
Enter the hydrochloric acid 20ml of 1mol/L, stirring is dissolved it, is transferred in 100ml volumetric flasks, add water and be settled to scale, shakes up, and stands
30min；Precision is measured in 5.0ml to 100ml volumetric flasks, is diluted with water to scale；Precision measures 10.0ml from dilution again
Into 100ml volumetric flasks, add 4ml lanthanums solution and be diluted with water to scale, shake up, upper machine is determined.Do reagent blank simultaneously.
The preparation of standards calibration curve：
Magnesium standard liquid 0,0.5,1.0,1.5,2.0,2.5ml is taken in 100ml volumetric flasks, 4ml lanthanum solution is separately added into, is diluted with water
It is settled to scale；Mix, upper machine.Test data is shown in Table 1, Fig. 1.
The magnesium density of table 1 and absorbance data table
Wherein, key instrument and reagent：Atomic absorption spectrophotometer：TAS-990 types；Electronic analytical balance：AL-204 types；Salt
Acid：Top pure grade；Lanthanum solution：58.7g lanthanas are weighed to be placed in 1000ml volumetric flasks, plus a small amount of water moistening, add hydrochloric acid
250ml dissolves it and is settled to scale, stores standby.
The configuration of magnesium standard liquid：Precision measures magnesium Standard Stock solutions（1000ug/ml）In 1.0ml to 50ml volumetric flasks, plus
Enter 1mol/L hydrochloric acid 5ml, add water and be settled to scale.Experimental water is ultra-pure water
The instrument condition of work is as follows：Spectral bandwidth：0.4nm, negative high voltage 589.50V, lamp current 2.0mA, gas flow
1500mL/min, burner height 6.0nm, burner position 5.0nm, wavelength 285.2nm, measuring method flame absorb.
The beneficial effects of the present invention are：The present invention prepares test fluid, NITRATE BY FLAME ATOMIC using sour sample dissolution, lanthanum salt solution
Absorption spectrophotometry determines content of magnesium method in omeprazole magnesium crude medicine, through Method validation, with preferable precision and standard
True property.
Brief description of the drawings
Fig. 1 is the standard curve collection of illustrative plates of magnesium of the present invention.
Specific embodiment
Specific embodiment of the invention is illustrated below in conjunction with the accompanying drawings：
Embodiment 1：
The treatment of sample：
Need testing solution：It is accurate to weigh the uniform sample 0.2500g of crushing（It is accurate to 0.0001g）It is placed in 50ml beakers, plus
Enter the hydrochloric acid 20ml of 1mol/L, stirring is dissolved it, is transferred in 100ml volumetric flasks, add water and be settled to scale, shakes up, and stands
30min；Precision is measured in 5.0ml to 100ml volumetric flasks, is diluted with water to scale；Precision measures 10.0ml from dilution again
Into 100ml volumetric flasks, add 4ml lanthanums solution and be diluted with water to scale, shake up, upper machine is determined.Do reagent blank simultaneously.Profit
Magnesium standard curve is used, content of magnesium is determined using atomic absorption spectrophotometer.
Instrument condition of work is as follows：Spectral bandwidth：0.4nm, negative high voltage 589.50V, lamp current 2.0mA, gas flow
1500mL/min, burner height 6.0nm, burner position 5.0nm, wavelength 285.2nm, measuring method flame absorb.
（1）Precision Experiment
Take with batch sample as examination with computer liquid, METHOD FOR CONTINUOUS DETERMINATION 6 times, with dry product content of magnesium（%）Represent and calculate, as a result show,
Relative standard deviation is 0.12%, and determination data the results are shown in Table 2.
The magnesium precision determination data result of table 2
（2）Intermediate precision
With same batch of sample, different personnel's different times determine precision, and method has preferable Intermediate precision.Detection data knot
Fruit such as table 3.
The magnesium Intermediate precision determination data result of table 3
（3）Test limit is tested
Precision measures 4ml lanthanum solution, is diluted with water to 100ml, and the solution is determined 20 times as machine on blank solution, with 20 blank
Value 3 times of corresponding concentration of standard deviation are used as test limit.Test limit measurement result=3*SD/K（SD：Standard deviation, K:Standard is bent
Line slope）.Determination data the results are shown in Table 4.
The test limit measured data result of table 4
（4）The rate of recovery is tested
6 parts are weighed with batch sample 0.2500g (being accurate to 0.0001g) left and right sample, the magnesium standard inventory for being separately added into equivalent is molten
Liquid 4ml, is processed by this experiment process method, and measurement result is shown in Table 5.
The magnesium recovery of standard addition experimental result of table 5
Result shows that 99.2%~103.5%, the method has preferably accurate magnesium recovery of standard addition.
（5）Sample size determination test
Three batches of sample content of magnesium of self-control, measurement result such as table 6 below are determined according to this law.
The sample content of magnesium measurement result of table 6
| Lot number | Content of magnesium % |
| 1 | 3.35 |
| 2 | 3.37 |
| 3 | 3.37 |
Comparative example 1：Experimental technique is same as Example 1, and it is 0.5mol/L to differ only in sample and add concentration of hydrochloric acid, carries out essence
Density and the rate of recovery are tested.
Comparative example 2：Experimental technique is same as Example 1, and it is 2mol/L to differ only in sample and add concentration of hydrochloric acid, is carried out
Precision and the rate of recovery are tested.
Comparative example 3：Experimental technique is same as Example 1, and it is 10ml to differ only in sample and add hydrochloric acid, carries out precision
Tested with the rate of recovery.
Comparative example 4：Experimental technique is same as Example 1, and it is 30ml to differ only in sample and add hydrochloric acid, carries out precision
Tested with the rate of recovery.Result such as following table：
Result shows：The relative standard deviation of the magnesium that the method for embodiment 1 is determined is substantially less than comparative example 1-4, average recovery rate
It is significantly higher than comparative example 1-4（p<0.05）, error is small, and accuracy is good.
The measurement result of table 7 is compared
| Project | Magnesium relative standard deviation | Average recovery rate |
| Embodiment 1 | 0.12% | 101.5% |
| Comparative example 1 | 0.55% | 90.2% |
| Comparative example 2 | 0.62% | 91.5% |
| Comparative example 3 | 0.33% | 93.0% |
| Comparative example 4 | 0.40% | 90.9% |
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art,
On the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications should also be regarded
It is protection scope of the present invention.
Claims (3)
1. it is a kind of determine omeprazole magnesium crude medicine in content of magnesium method, it is characterised in that methods described include following step
Suddenly：Sample pre-treatments are first carried out, magnesium standard curve is then prepared, content of magnesium is determined using atomic absorption spectrophotometry；
Atomic absorption spectrophotometer condition of work wherein used is：Spectral bandwidth：0.4nm, negative high voltage 589.50V, lamp current
2.0mA, gas flow 1500mL/min, burner height 6.0nm, burner position 5.0nm, wavelength 285.2nm.
2. the method for determining the content of magnesium in omeprazole magnesium crude medicine as claimed in claim 1, it is characterised in that before sample
Processing method is as follows：
The accurate uniform sample 0.2500g of crushing that weighs is placed in 50ml beakers, adds the hydrochloric acid 20ml of 1mol/L, and stirring makes it
Dissolving, is transferred in 100ml volumetric flasks, adds water and is settled to scale, shakes up, and stands 30min；Precision measures 5.0ml to 100ml appearances
In measuring bottle, scale is diluted with water to；During precision measures 10.0ml to 100ml volumetric flasks from dilution again, 4ml lanthanum solution is added
And scale is diluted with water to, and shaking up, upper machine is determined；Do reagent blank simultaneously；Wherein lanthanum solution manufacturing method is as follows：Weigh
58.7g lanthanas are placed in 1000ml volumetric flasks, plus a small amount of water moistening, and adding hydrochloric acid 250ml dissolves it and be settled to quarter
Degree, stores standby.
3. the method for determining the content of magnesium in omeprazole magnesium crude medicine as claimed in claim 2, it is characterised in that magnesium standard
The preparation method of curve is as follows：Magnesium standard liquid is configured first, and precision measures 1000ug/ml magnesium Standard Stock solutions 1.0ml to 50ml
In volumetric flask, 1mol/L hydrochloric acid 5ml are added, add water and be settled to scale, experimental water is ultra-pure water；Next takes magnesium standard liquid 0,0.5,
1.0,1.5,2.0,2.5ml in 100ml volumetric flasks, are separately added into 4ml lanthanum solution, are diluted with water and are settled to scale；Mix, on
Machine；Magnesium standard curve is made finally according to measurement result.
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| CN201710178335.6A CN106769953A (en) | 2017-03-23 | 2017-03-23 | A kind of method of the content of magnesium in measure omeprazole magnesium crude medicine |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101566561A (en) * | 2009-05-26 | 2009-10-28 | 上海大学 | Method for measuring microelement in radish |
| CN101701962A (en) * | 2009-11-19 | 2010-05-05 | 首都医科大学附属北京朝阳医院 | Serum magnesium standard substance |
| CN103175802A (en) * | 2011-12-20 | 2013-06-26 | 四川科伦药物研究有限公司 | Method for determining content of magnesium element in hydroxyethyl starch injection preparation |
| CN106338477A (en) * | 2016-10-14 | 2017-01-18 | 内蒙古天奇中蒙制药股份有限公司 | Method for quick detection of contents of microelements in xuefuzhuyu pills |
-
2017
- 2017-03-23 CN CN201710178335.6A patent/CN106769953A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101566561A (en) * | 2009-05-26 | 2009-10-28 | 上海大学 | Method for measuring microelement in radish |
| CN101701962A (en) * | 2009-11-19 | 2010-05-05 | 首都医科大学附属北京朝阳医院 | Serum magnesium standard substance |
| CN103175802A (en) * | 2011-12-20 | 2013-06-26 | 四川科伦药物研究有限公司 | Method for determining content of magnesium element in hydroxyethyl starch injection preparation |
| CN106338477A (en) * | 2016-10-14 | 2017-01-18 | 内蒙古天奇中蒙制药股份有限公司 | Method for quick detection of contents of microelements in xuefuzhuyu pills |
Non-Patent Citations (1)
| Title |
|---|
| 张艳红: ""埃索美拉唑镁中镁的含量测定方法研究"", 《科技研究——2015科技产业发展与建设成就研讨会论文集》 * |
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Application publication date: 20170531 |