CN106290619A - A kind of child ties up the detection method of vitamin d3 levels in D Biocal preparation - Google Patents
A kind of child ties up the detection method of vitamin d3 levels in D Biocal preparation Download PDFInfo
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- CN106290619A CN106290619A CN201610612293.8A CN201610612293A CN106290619A CN 106290619 A CN106290619 A CN 106290619A CN 201610612293 A CN201610612293 A CN 201610612293A CN 106290619 A CN106290619 A CN 106290619A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The present invention provides a kind of child to tie up the detection method of vitamin d3 levels in D Biocal preparation.The method uses high performance liquid chromatography to carry out, and comprises the steps: that (1) preparation child ties up D Biocal sample solution；(2) step (1) gained sample solution is injected high performance liquid chromatograph, use flowing to carry out isocratic elution mutually, and record chromatograph；Wherein, described performance liquid chromatographic column fixes phase filler is amino chemically bonded silica；Flowing phase be formulated as normal hexane isopropanol (99: 1).The detection method of the present invention measures vitamin D3 under same liquid-phase condition, and described detection method is easy and simple to handle, separating degree is high, assay method specificity is strong, testing result is the most credible.
Description
Technical field
The invention belongs to pharmaceutical analysis field, specifically, the present invention relates to a kind of child and tie up dimension in D Biocal preparation
The detection method of raw element D3 content.
Background technology
It is a kind of for children calcium supplement that child ties up D Biocal, and child ties up needed for D Biocal can supplement child
Calcium, is administered orally for calcium replenishing agent, wherein can contain vitamin D3, but current that detection method operates responsible, testing result
Accuracy is low.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, it is provided that a kind of child ties up D Biocal system
The detection method of vitamin d3 levels in agent.
In order to solve above-mentioned technical problem, the invention provides following technical scheme: a kind of child ties up D Biocal system
The detection method of vitamin d3 levels in agent, the method uses high performance liquid chromatography to carry out, comprises the steps:
(1) preparation child ties up D Biocal sample solution, and described child ties up D Biocal sample solution and includes need testing solution
And reference substance solution；
(2) step (1) gained sample solution is injected high performance liquid chromatograph, carry out isocratic elution mutually with flowing, and record color
Spectrogram；
Wherein, the preparation of described need testing solution comprise the steps: to take this product 25 (specification every calcium carbonate 0.75 gram,
Be equivalent to calcium 0.3 gram；Vitamin D3100 ius (2.5 microgram)), accurately weighed, calculate average tablet weight, finely ground, accurate title
Take fine powder appropriate (being approximately equivalent to vitamin D3 25 μ g), put in 100ml brown measuring bottle, add solution [with dimethyl sulfoxide-water (10
: 2) mixed solution makes in every 1ml containing the solution of 2,6 ditertiary butyl p cresol (BHT) 0.2mg] 50ml, the ultrasonic place of ice-water bath
Managing 15 minutes, and shake constantly, keep ultrasonic water bath temperature less than 30 DEG C, precision adds the hexane solution of 0.02%BHT
25ml, after shaking 15 minutes, less than 30 DEG C centrifugal 5 minutes (4000rpm), and to divide and take upper solution, lucifuge obtains clear after standing 1 hour
Clear solution is as need testing solution；Precision measures need testing solution 500 μ l, injects chromatograph of liquid, records chromatogram；
The chromatographic column fixed phase filler amino chemically bonded silica of described high performance liquid chromatography；
Being formulated as of flowing phase: normal hexane-isopropanol (99: 1).
Preferably, the eluting order of described high performance liquid chromatography is as follows:
Flowing 100% volume mutually when 0-15 minute.
Preferably, the flow velocity of described flowing phase is 1.5ml/min.
Preferably, the chromatographic column column temperature of described high performance liquid chromatography is 25-35 DEG C, and detection wavelength is 265nm.
Preferably, in high performance liquid chromatography detecting step (2), first contrast solution is injected chromatograph of liquid, adjust
Joint detector sensitivity, makes peak height is monitor full scale the 50% of main constituent chromatographic peak；Again by need testing solution and impurity
Sample-adding solution is injected separately into chromatograph of liquid, uses flowing to carry out isocratic elution mutually, and records chromatogram, injects chromatograph of liquid
The amount of middle sample solution is 500 μ l.
Preferably, the chromatographic column column temperature of described high performance liquid chromatography is 30 DEG C.
The detection method of the present invention measures vitamin D3 under same liquid-phase condition, described detection method is easy and simple to handle, point
From degree height, assay method specificity is strong, testing result is the most credible.
Embodiment
Embodiment 1
(1) preparation child ties up D Biocal sample solution, and described child ties up D Biocal sample solution and includes need testing solution
And reference substance solution；
(2) step (1) gained sample solution is injected high performance liquid chromatograph, carry out isocratic elution mutually with flowing, and record color
Spectrogram；
Wherein, the preparation of described need testing solution comprise the steps: to take this product 25 (specification every calcium carbonate 0.75 gram,
Be equivalent to calcium 0.3 gram；Vitamin D3100 ius (2.5 microgram)), accurately weighed, calculate average tablet weight, finely ground, accurate title
Take fine powder appropriate (being approximately equivalent to vitamin D3 25 μ g), put in 100ml brown measuring bottle, add solution [with dimethyl sulfoxide-water (10
: 2) mixed solution makes in every 1ml containing the solution of 2,6 ditertiary butyl p cresol (BHT) 0.2mg] 50ml, the ultrasonic place of ice-water bath
Managing 15 minutes, and shake constantly, keep ultrasonic water bath temperature less than 30 DEG C, precision adds the hexane solution of 0.02%BHT
25ml, after shaking 15 minutes, less than 30 DEG C centrifugal 5 minutes (4000rpm), and to divide and take upper solution, lucifuge obtains clear after standing 1 hour
Clear solution is as need testing solution；Precision measures need testing solution 500 μ l, injects chromatograph of liquid, records chromatogram；
The chromatographic column fixed phase filler amino chemically bonded silica of described high performance liquid chromatography；
Being formulated as of flowing phase: normal hexane-isopropanol (99: 1).
Claims (6)
1. a detection method for vitamin d3 levels during child ties up D Biocal preparation, in wherein said dimension D Biocal
Effective ingredient includes vitamin D3, and the method uses high performance liquid chromatography to carry out, it is characterised in that include following step
Rapid:
(1) preparation child ties up D Biocal sample solution, and described child ties up D Biocal sample solution and includes need testing solution
And reference substance solution；
(2) step (1) gained sample solution is injected high performance liquid chromatograph, carry out isocratic elution mutually with flowing, and record color
Spectrogram；
Wherein, the preparation of described need testing solution comprise the steps: to take this product 25 (specification every calcium carbonate 0.75 gram,
Be equivalent to calcium 0.3 gram；Vitamin D3100 ius (2.5 microgram)), accurately weighed, calculate average tablet weight, finely ground, accurate title
Take fine powder appropriate (being approximately equivalent to vitamin D3 25 μ g), put in 100ml brown measuring bottle, add solution [with dimethyl sulfoxide-water (10
: 2) mixed solution makes in every 1ml containing the solution of 2,6 ditertiary butyl p cresol (BHT) 0.2mg] 50ml, the ultrasonic place of ice-water bath
Managing 15 minutes, and shake constantly, keep ultrasonic water bath temperature less than 30 DEG C, precision adds the hexane solution of 0.02%BHT
25ml, after shaking 15 minutes, less than 30 DEG C centrifugal 5 minutes (4000rpm), and to divide and take upper solution, lucifuge obtains clear after standing 1 hour
Clear solution is as need testing solution；Precision measures need testing solution 500 μ l, injects chromatograph of liquid, records chromatogram；
The chromatographic column fixed phase filler amino chemically bonded silica of described high performance liquid chromatography；
Being formulated as of flowing phase: normal hexane-isopropanol (99: 1).
The detection method of method the most according to claim 1, it is characterised in that the eluting order of described high performance liquid chromatography
As follows:
Flowing 100% volume mutually when 0-15 minute.
The detection method of method the most according to claim 1, it is characterised in that the flow velocity of described flowing phase is 1.5ml/min.
The detection method of method the most according to claim 1, it is characterised in that the chromatographic column post of described high performance liquid chromatography
Temperature is 25-35 DEG C, and detection wavelength is 265nm.
The detection method of method the most according to claim 1, it is characterised in that in high performance liquid chromatography detecting step (2)
In, first contrast solution being injected chromatograph of liquid, regulates detector sensitivity, the peak height making main constituent chromatographic peak is monitor
The 50% of full scale；Again need testing solution and impurity are loaded solution and are injected separately into chromatograph of liquid, use flowing to carry out mutually
Degree eluting, and record chromatogram, the amount of sample solution in chromatograph of liquid of injecting is 500 μ l.
The detection method of method the most according to claim 4, it is characterised in that the chromatographic column post of described high performance liquid chromatography
Temperature is 30 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610612293.8A CN106290619A (en) | 2016-07-31 | 2016-07-31 | A kind of child ties up the detection method of vitamin d3 levels in D Biocal preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610612293.8A CN106290619A (en) | 2016-07-31 | 2016-07-31 | A kind of child ties up the detection method of vitamin d3 levels in D Biocal preparation |
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|---|---|
| CN106290619A true CN106290619A (en) | 2017-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610612293.8A Pending CN106290619A (en) | 2016-07-31 | 2016-07-31 | A kind of child ties up the detection method of vitamin d3 levels in D Biocal preparation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760919A (en) * | 2018-05-28 | 2018-11-06 | 广州富诺健康科技股份有限公司 | A kind of children tie up the detection method of vitamin d3 levels in D Biocal preparations |
| CN109709237A (en) * | 2018-12-07 | 2019-05-03 | 浙江核力欣健药业有限公司 | A kind of calcium carbonate D3The related substance detecting method of chewable tablets |
| CN114088826A (en) * | 2021-10-27 | 2022-02-25 | 昆明源瑞制药有限公司 | Extraction method of vitamin D3 and method for detecting content of vitamin D3 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103869024A (en) * | 2014-04-04 | 2014-06-18 | 贵州联盛药业有限公司 | Method for detecting content of vitamin D3 in infant calcium carbonate D3 granule |
| CN104502501A (en) * | 2014-12-26 | 2015-04-08 | 江苏艾兰得营养品有限公司 | Chromatographic method for rapidly measuring content of vitamin D3 |
| CN105372337A (en) * | 2014-08-07 | 2016-03-02 | 山东达因海洋生物制药股份有限公司 | Method for detecting vitamin D content in vitamin D drop |
-
2016
- 2016-07-31 CN CN201610612293.8A patent/CN106290619A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103869024A (en) * | 2014-04-04 | 2014-06-18 | 贵州联盛药业有限公司 | Method for detecting content of vitamin D3 in infant calcium carbonate D3 granule |
| CN105372337A (en) * | 2014-08-07 | 2016-03-02 | 山东达因海洋生物制药股份有限公司 | Method for detecting vitamin D content in vitamin D drop |
| CN104502501A (en) * | 2014-12-26 | 2015-04-08 | 江苏艾兰得营养品有限公司 | Chromatographic method for rapidly measuring content of vitamin D3 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760919A (en) * | 2018-05-28 | 2018-11-06 | 广州富诺健康科技股份有限公司 | A kind of children tie up the detection method of vitamin d3 levels in D Biocal preparations |
| CN109709237A (en) * | 2018-12-07 | 2019-05-03 | 浙江核力欣健药业有限公司 | A kind of calcium carbonate D3The related substance detecting method of chewable tablets |
| CN114088826A (en) * | 2021-10-27 | 2022-02-25 | 昆明源瑞制药有限公司 | Extraction method of vitamin D3 and method for detecting content of vitamin D3 |
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