CN106770207A - A kind of method of Trace Potassium and titanium in measure magnesium omeprazole - Google Patents
A kind of method of Trace Potassium and titanium in measure magnesium omeprazole Download PDFInfo
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- CN106770207A CN106770207A CN201710178334.1A CN201710178334A CN106770207A CN 106770207 A CN106770207 A CN 106770207A CN 201710178334 A CN201710178334 A CN 201710178334A CN 106770207 A CN106770207 A CN 106770207A
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- titanium
- potassium
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- magnesium omeprazole
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The method of a kind of Trace Potassium determined in magnesium omeprazole of the invention and titanium is related to inductive coupling plasma emission spectrum method（ICP）Determine residual minim potassium and Ti content in magnesium omeprazole, by the treatment of sample, the configuration of standards calibration curve solution, the method Accurate Determining residual minim potassium and Ti content of the content for drawing calibration curve, measure potassium and titanium, optimal Operating parameters are determined, method sensitivity for analysis is high, accuracy is high, simple with sample handling processes, reduces 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 Trace Potassium and the method for titanium in a kind of magnesium omeprazole, belong to analysis method field.
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.Need to be used to titanium salt and potassium according to magnesium omeprazole synthesis process
Salt, thus control detection magnesium omeprazole into the titanium and the content of potassium of residual be necessary quality index.The present invention have studied and adopt
Use inductively coupled plasma emission spectrometry（ICP）Determine in magnesium omeprazole residual minim potassium and Ti content and carry out method
Learn research.Purpose is to overcome method disunity in the prior art, and sensitivity is not high, disturbs larger 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
The method that medicine control process provides the Trace Potassium determined in magnesium omeprazole and titanium of accurate data.
The described method comprises the following steps：
Step one：The treatment of sample；
By sample comminution, be well mixed, accurately weigh sample as in polytetrafluoroethylene (PTFE) counteracting tank, add concentrated nitric acid, make acid and
Sample is fully mixed, and installs counteracting tank, and setting suitable parameter carries out micro-wave digestion.It is automatic cold after EP (end of program) is cleared up
But, counteracting tank is taken out, electricity consumption heater plate catches up with acid.Digestion solution water is settled in volumetric flask, while doing reagent blank；
Step 2：The configuration of standards calibration curve solution；
Potassium, titanium mix the configuration of standard liquid：The titanium standard liquid of 1ml is taken, 100ml is settled to water, then take the dilution of 10ml respectively
Titanium standard liquid afterwards and the potassium standard liquid of 4ml, as the volumetric flask of 100ml in, be settled to 100ml with water；Wherein potassium, titanium standard
Solution liquid：1000ug/ml；Experimental water is ultra-pure water；
Step 3：Draw calibration curve；
Standards calibration curve solution and blank sample solution are introduced into inductive coupling plasma emission spectrograph, determine it is to be measured from
The signal intensity of son, with mass-volume concentration as abscissa, the signal intensity of ion is ordinate drafting potassium and titanium calibration curve；
Step 4：Determine the content of potassium and titanium；
Specimen sample solution and blank sample solution are introduced into inductive coupling plasma emission spectrograph, measure treats measured ion
Signal intensity, the standard liquid calibration curve according to step 3 obtains potassium and titanium in blank sample solution and specimen sample solution
Mass percent.
Wherein, the quality of magnesium omeprazole sample to be measured is 0.15-0.20g, adds concentrated nitric acid 3-5ml, is settled to water
50mL, it is preferred that concentrated nitric acid addition is 4ml.
Preferably, the Parameter Conditions of the inductively coupled plasma emission spectrography are：Power：1450W；Atomization gas
Flow：0.78 L/min；Cooling gas flow：12.00 L/min；Auxiliary gas flow amount：0.80 L/min；Revolution speed：30 r/
min；Sample injection time：45 s .
The preparation of potassium and titanium blended standard curve：
Potassium is taken, titanium mixes standard liquid 0,0.5,2,5,10,20,40ml in 100ml volumetric flasks, adds dilution to be settled to scale.It is mixed
It is even.Upper machine.Such as following table linear equation measurement result.
The potassium concn of table 1 and intensity data table
The titanium concentration of table 2 and intensity data table
The beneficial effects of the present invention are：The present invention uses inductive coupling plasma emission spectrum method（ICP）Determine Omeprazole
Residual minim potassium and Ti content in magnesium, it is determined that optimal Operating parameters, sensitivity for analysis is high, and accuracy is high, and sample
Processing procedure is simple, reduces the disturbing factor in determining, the advantages of operability is good.
Brief description of the drawings
Fig. 1 is the standard curve collection of illustrative plates of potassium of the present invention.
Fig. 2 is the standard curve collection of illustrative plates of titanium of the present invention.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1：
By sample comminution, it is well mixed, accurately weighs 0.15-0.20g samples as in polytetrafluoroethylene (PTFE) counteracting tank, adds dense nitre
Sour 4ml, makes acid and sample fully mix, and installs counteracting tank, and setting suitable parameter carries out micro-wave digestion.Program knot to be cleared up
Cooled down automatically after beam, take out counteracting tank, electricity consumption heater plate catches up with acid.Digestion solution water is settled in the volumetric flask of 50ml,
Do reagent blank simultaneously.
Sample solution and blank sample solution are introduced into inductive coupling plasma emission spectrograph, measure treats measured ion
Signal intensity, according to standard liquid calibration curve, obtains the quality hundred of potassium and titanium in blank sample solution and specimen sample solution
Fraction, obtains the content of surveyed potassium and titanium.
The Parameter Conditions of the inductively coupled plasma emission spectrography are：Power：1450W；Atomization gas flow：
0.78 L/min；Cooling gas flow：12.00 L/min；Auxiliary gas flow amount：0.80 L/min；Revolution speed：30 r/min；
Sample injection time：45 s .
（1）Precision Experiment：
The sample of same lot number is taken as examination with computer liquid, instrument stabilizer is treated, METHOD FOR CONTINUOUS DETERMINATION 6 times represents calculating with content.As a result
Show, potassium relative standard deviation 0.78%.Titanium relative standard deviation 0.83%, determination data the results are shown in Table 3.
The precision determination data result of table 3
| Project | 1 | 2 | 3 | 4 | 5 | 6 | Average value | RSD（%） |
| Potassium | 45.79 | 46.66 | 46.32 | 46.19 | 45.97 | 45.70 | 46.10 | 0.78 |
| Titanium | 148.89 | 146.58 | 148.89 | 149.74 | 147.57 | 147.05 | 148.12 | 0.83 |
（2）Intermediate precision is tested：
With same batch of sample, different personnel's different times measure precision, statistics such as table 4 below.
The Intermediate precision experimental result of table 4
（3）Test limit is tested：
To in polytetrafluoroethylene (PTFE) counteracting tank, concentrated nitric acid 4ml is added, install counteracting tank, carried out with Specimen eliminating identical parameter
Micro-wave digestion, machine on final constant volume solution is determined 20 times；Using 20 blank value standard deviations, 3 times of corresponding concentration as detection
Limit.Test limit computing formula is as follows, and test result is shown in Table 5.
Test limit measurement result=3*SD/K（SD：Standard deviation, K:Slope of standard curve）
The potassium of table 5, titanium test limit result
（4）Sample size determination test
The content of three batches of sample potassium and titanium, measurement result such as table 6 below are determined according to this law.
The sample potassium of table 6 and Ti content measurement result
| Lot number | Potassium content（mg/kg） | Ti content (mg/kg) |
| 1 | 289.1 | 74.5 |
| 2 | 300.0 | 46.8 |
| 3 | 296.0 | 66.1 |
（5）The rate of recovery is tested：
6 parts of samples of lot number are weighed, and same amount of potassium and titanium standard liquid are separately added into sample, according to this experiment
Method carrys out determination sample recovery of standard addition, and test result is shown in Table 7.
The potassium of table 7 and titanium recovery of standard addition experimental result
Result shows, potassium determines recovery of standard addition between 95.40%~102.17%, titanium determine recovery of standard addition 97.50%~
Between 98.80%, the method has preferable accuracy.
Comparative example 1：Experimental technique is same as Example 1, differs only in addition concentrated nitric acid 1ml, carries out Precision Experiment.
Comparative example 2：Experimental technique is same as Example 1, differs only in addition concentrated nitric acid 3ml, carries out Precision Experiment.
Comparative example 3：Experimental technique is same as Example 1, differs only in addition concentrated nitric acid 5ml, carries out Precision Experiment.
Comparative example 4：Experimental technique is same as Example 1, differs only in addition concentrated nitric acid 7ml, carries out Precision Experiment.
Result such as following table：
Result shows：The potassium and the relative standard deviation of titanium that the method for embodiment 1 is determined are substantially less than comparative example 1-4（p<
0.05）, the method is optimal Operating parameters, and error is small, and accuracy is high.
The measurement result of table 8 is compared
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 (4)
1. Trace Potassium in a kind of measure magnesium omeprazole and the method for titanium, it is characterised in that the described method comprises the following steps：
Step one：The treatment of sample；
By sample comminution, be well mixed, accurately weigh sample as in polytetrafluoroethylene (PTFE) counteracting tank, add concentrated nitric acid, make acid and
Sample is fully mixed, and installs counteracting tank, and setting suitable parameter carries out micro-wave digestion, automatic cold after EP (end of program) is cleared up
But, counteracting tank is taken out, electricity consumption heater plate catches up with acid, digestion solution water is settled in volumetric flask, while doing reagent blank；
Step 2：The configuration of standards calibration curve solution；
Potassium, titanium mix the configuration of standard liquid：The titanium standard liquid of 1ml is taken, 100ml is settled to water, then take the dilution of 10ml respectively
Titanium standard liquid afterwards and the potassium standard liquid of 4ml, as the volumetric flask of 100ml in, be settled to 100ml with water；Wherein potassium, titanium standard
Solution liquid is 1000ug/ml；Experimental water is ultra-pure water；
Step 3：Draw calibration curve；
Standards calibration curve solution and blank sample solution are introduced into inductive coupling plasma emission spectrograph, determine it is to be measured from
The signal intensity of son, with mass-volume concentration as abscissa, the signal intensity of ion is ordinate drafting potassium and titanium calibration curve；
Step 4：Determine the content of potassium and titanium；
Specimen sample solution and blank sample solution are introduced into inductive coupling plasma emission spectrograph, measure treats measured ion
Signal intensity, the standard liquid calibration curve according to step 3 obtains potassium and titanium in blank sample solution and specimen sample solution
Mass percent, obtain the content of surveyed potassium and titanium.
2. Trace Potassium in measure magnesium omeprazole as claimed in claim 1 and the method for titanium, it is characterised in that the step
The quality of magnesium omeprazole sample to be measured is 0.15-0.20g in one, adds concentrated nitric acid 3-5ml, is settled to 50mL with water.
3. Trace Potassium in measure magnesium omeprazole as claimed in claim 2 and the method for titanium, it is characterised in that the step
The quality of magnesium omeprazole sample to be measured is 0.15-0.20g in one, adds concentrated nitric acid 4ml, is settled to 50mL with water.
4. Trace Potassium in measure magnesium omeprazole as claimed in claim 1 and the method for titanium, it is characterised in that the inductance
The Parameter Conditions of coupled plasma optical emission spectroscopic methodology are：Power：1450W；Atomization gas flow：0.78 L/min；Cooling gas
Body flow：12.00 L/min；Auxiliary gas flow amount：0.80 L/min；Revolution speed：30 r/min；Sample injection time：45s .
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Citations (4)
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| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
| CN101308065A (en) * | 2008-07-03 | 2008-11-19 | 攀钢集团研究院有限公司 | Titanium dioxide resolving method and detection method |
| CN103630599A (en) * | 2013-01-09 | 2014-03-12 | 威海出入境检验检疫局检验检疫技术中心 | Method for measuring potassium content in humic acid and humates by ICP-MS |
| CN105510301A (en) * | 2016-02-14 | 2016-04-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring aluminum, magnesium, calcium, vanadium, titanium, nickel, copper and manganese in rare earth silicon-magnesium alloy |
-
2017
- 2017-03-23 CN CN201710178334.1A patent/CN106770207A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101308065A (en) * | 2008-07-03 | 2008-11-19 | 攀钢集团研究院有限公司 | Titanium dioxide resolving method and detection method |
| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
| CN103630599A (en) * | 2013-01-09 | 2014-03-12 | 威海出入境检验检疫局检验检疫技术中心 | Method for measuring potassium content in humic acid and humates by ICP-MS |
| CN105510301A (en) * | 2016-02-14 | 2016-04-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring aluminum, magnesium, calcium, vanadium, titanium, nickel, copper and manganese in rare earth silicon-magnesium alloy |
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| 刘晶 等: "微波消解和电感耦合等离子体发射光谱法同时测定煤灰中的14种元素", 《分析化学》 * |
| 姜鹰雁 等: "电感耦合等离子体原子发射光谱法测定艾司奥美拉唑镁中镁的含量", 《中国药师》 * |
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Application publication date: 20170531 |