CN105974035A - Method for detecting content of vitamin D3 in vitamin D calcium chewable tablet preparation - Google Patents
Method for detecting content of vitamin D3 in vitamin D calcium chewable tablet preparation Download PDFInfo
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- CN105974035A CN105974035A CN201610612209.2A CN201610612209A CN105974035A CN 105974035 A CN105974035 A CN 105974035A CN 201610612209 A CN201610612209 A CN 201610612209A CN 105974035 A CN105974035 A CN 105974035A
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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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- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention relates to a method for detecting the content of vitamin D3 in a vitamin D calcium chewable tablet preparation. The method comprises the steps that firstly, a vitamin D calcium chewable tablet sample solution is prepared; secondly, the sample solution obtained in the first step is injected into a high-performance liquid chromatograph, a mobile phase is used for carrying out isocratic elution, and color spectra are recorded. According to the detecting method, relative substances in Ambrisentan raw materials or preparations are detected under the same liquid phase condition, and the detecting method is easy and convenient to implement, high in separation degree, high in specificity and accurate and credible in detection result.
Description
Technical field
The invention belongs to pharmaceutical analysis field.Specifically, the present invention relates to a kind of use the detection method of vitamin d3 levels in high effective liquid chromatography for measuring dimension D Biocal preparation.
Background technology
Dimension D Biocal is by a kind of adult's calcium complement agent of ounce pharmaceutical Co. Ltd of U.S. exploitation, English language Chemical name: Calcium Supplement with Vitamin D
Chewable Tablets, chemical constitution is as follows: its molecular weight is 384, and molecular formula is (C27H44O).Dimension D Biocal can supplement the calcium of needed by human body, is administered orally for calcium replenishing agent, and (specification every calcium carbonate 0.75 gram is equivalent to calcium 0.3 gram to the conventional tablet that has of listing at present；Vitamin D3 100 iu (2.5 microgram)).
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 tie up the detection method of vitamin d3 levels in D Biocal preparation.
In order to solve above-mentioned technical problem, the invention provides following technical scheme: a kind of 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:
(1) preparation dimension D Biocal sample solution, described dimension D Biocal sample solution 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 chromatogram；Wherein, the preparation of described need testing solution comprises the steps: to take this product 25, accurately weighed, calculate average tablet weight, finely ground, it is appropriate (being approximately equivalent to vitamin D3 25 μ g) that precision weighs fine powder, put in 100ml brown measuring bottle, add solution 50ml, solution dimethyl sulfoxide-water (10: 2) mixed solution is made in every 1ml containing 2, the solution of 6-ditertbutylparacresol (BHT) 0.2mg, ice-water bath supersound process 15 minutes, and shake constantly, keep ultrasonic water bath temperature less than 30 DEG C, the accurate hexane solution 25ml adding 0.02%BHT, after shaking 15 minutes, less than 30 DEG C centrifugal 5 minutes (4000rpm), divide and take upper solution, lucifuge obtains settled solution as need testing solution after standing 1 hour；Precision measures need testing solution 500 μ l, injects chromatograph of liquid, records chromatogram, wherein the chromatographic column fixed phase filler amino chemically bonded silica of 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 such as: 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, the chromatographic column column temperature of described high performance liquid chromatography is 30 DEG C.
Preferably, in high performance liquid chromatography detecting step (2), first contrast solution is injected chromatograph of liquid, regulate detector sensitivity, make peak height is monitor full scale the 50% of main constituent chromatographic peak；Again need testing solution and impurity are loaded solution and are injected separately into chromatograph of liquid, use flowing to carry out isocratic elution mutually, and record chromatogram；Preferably, the amount of sample solution in chromatograph of liquid of injecting is 500 μ l.
The detection method of the present invention measures the related substance that has in ambrisentan raw material or preparation 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.
Detailed description of the invention
Embodiment 1
[assay] vitamin D3 measures according to high performance liquid chromatography (Chinese Pharmacopoeia two annex V D of version in 2010).
Chromatographic condition and system suitability: be filler (Sepax HP-Amino is the most applicable) with amino chemically bonded silica；With normal hexane-isopropanol (99: 1) for flowing phase；Flow velocity 1.5ml/min, detection wavelength is 265nm.Take reference substance solution in 60 DEG C of water-baths, heat 1 hour (making generation PreD3), let cool, measure 500 μ l and inject chromatograph of liquid, record chromatogram, the separating degree of vitamin D3 peak and PreD3 should be not less than 5, number of theoretical plate is calculated by vitamin D3 peak should be not less than 5000, and tailing factor should be not more than 2.0.
nullAlgoscopy: (lucifuge operation) takes this product 25，Accurately weighed，Finely ground，It is appropriate (being approximately equivalent to vitamin D3 25 μ g) that precision weighs fine powder，Put in 100ml brown measuring bottle，Add solution [to make in every 1ml containing 2 with dimethyl sulfoxide-water (10: 2) mixed solution,The solution of 6-ditertbutylparacresol (BHT) 0.2mg] 50ml，Ice-water bath supersound process 15 minutes，And shake constantly，Keep ultrasonic water bath temperature less than 30 DEG C，Precision adds the hexane solution 25ml of 0.02%BHT，After shaking 15 minutes，Centrifugal 5 minutes (4000rpm)，Divide and take upper solution，Lucifuge obtains settled solution as need testing solution after standing 1 hour，Precision measures need testing solution 500 μ l，Inject chromatograph of liquid，Record chromatogram；Separately take vitamin D3 reference substance appropriate, accurately weighed, dissolve with the hexane solution of 0.02%BHT and quantitatively the solution in every 1ml containing about 1 μ g is made in dilution, be measured in the same method, by external standard method with calculated by peak area.Result of calculation is multiplied by 1.09 and i.e. obtains vitamin d3 levels.Mensuration should darkroom and avoid oxidation in the case of carry out.
Calcium carbonate: the powder 0.24g(taking this product finely ground is approximately equivalent to calcium carbonate 150mg), accurately weighed, put in crucible, the most blazing to complete carbonization, then move to 700～800 DEG C of calcinations about 2 hours, let cool, residue adds water 10ml, dropping 3mol/L hydrochloric acid solution 2ml, heating makes residue in crucible be completely dissolved, is transferred in conical flask with water 100ml, add 1mol/L sodium hydroxide solution 15ml, make pH be more than 12, add hydroxynaphthol blue indicator solution 2, be titrated to solution with Calcium Disodium Versenate volumetric solution (0.05mol/L) and become pure blue from aubergine.Every 1ml Calcium Disodium Versenate volumetric solution (0.05mol/L) is equivalent to the CaCO3 of 5.004mg.
Claims (6)
1. tieing up a detection method for vitamin d3 levels in D Biocal preparation, the method uses high performance liquid chromatography to carry out, it is characterised in that comprise the steps:
(1) preparation dimension D Biocal sample solution, described dimension D Biocal sample solution 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 chromatogram；Wherein, the preparation of described need testing solution comprises the steps: to take this product 25, accurately weighed, calculate average tablet weight, finely ground, it is appropriate that precision weighs fine powder, put in 100ml brown measuring bottle, add solution 50ml, solution dimethyl sulfoxide-water mixed solution is made in every 1ml containing 2, the solution of 6-ditertbutylparacresol (BHT) 0.2mg, ice-water bath supersound process 15 minutes, and shake constantly, keep ultrasonic water bath temperature less than 30 DEG C, the accurate hexane solution 25ml adding 0.02%BHT, after shaking 15 minutes, less than 30 DEG C centrifugal 5 minutes (4000rpm), divide and take upper solution, lucifuge obtains settled solution as need testing solution after standing 1 hour；Precision measures need testing solution 500 μ l, injects chromatograph of liquid, records chromatogram, wherein the chromatographic column fixed phase filler amino chemically bonded silica of high performance liquid chromatography, being formulated as of flowing phase: normal hexane-isopropanol 99: 1.
Method the most according to claim 1, it is characterised in that the eluting order of described high performance liquid chromatography is such as: flowing 100% volume mutually when 0-15 minute.
Method the most according to claim 1, it is characterised in that the flow velocity of described flowing phase is 1.5ml/min.
Method the most according to claim 1, it is characterised in that the chromatographic column column temperature of described high performance liquid chromatography is 25-35 DEG C, detection wavelength is 265nm.
Method the most according to claim 1, it is characterised in that in high performance liquid chromatography detecting step (2), first injects chromatograph of liquid by contrast solution, regulates detector sensitivity, makes peak height is monitor full scale the 50% of main constituent chromatographic peak；Again need testing solution and impurity are loaded solution and are injected separately into chromatograph of liquid, use flowing to carry out isocratic elution mutually, and record chromatogram；Preferably, the amount of sample solution in chromatograph of liquid of injecting is 500 μ l.
Method the most according to claim 4, it is characterised in that the chromatographic column column temperature of described high performance liquid chromatography is 30 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109541110A (en) * | 2018-12-07 | 2019-03-29 | 浙江核力欣健药业有限公司 | A kind of detection children's calcium carbonate D3Vitamin D in particle3Method in relation to substance |
| 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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| 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 |
| CN105403631A (en) * | 2015-10-28 | 2016-03-16 | 浙江省疾病预防控制中心 | Method for rapidly detecting content of vitamin D3 in health foods |
-
2016
- 2016-07-31 CN CN201610612209.2A patent/CN105974035A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105403631A (en) * | 2015-10-28 | 2016-03-16 | 浙江省疾病预防控制中心 | Method for rapidly detecting content of vitamin D3 in health foods |
Non-Patent Citations (1)
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| 王乔飞: "HPLC法测定多维片中痕量维生素D3的含量", 《淮阴工学院学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109541110A (en) * | 2018-12-07 | 2019-03-29 | 浙江核力欣健药业有限公司 | A kind of detection children's calcium carbonate D3Vitamin D in particle3Method in relation to substance |
| 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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Application publication date: 20160928 |