CN102043024A - Method for measuring materials associated with huperzine A orally disintegrating tablets by high performance liquid chromatography (HPLC) - Google Patents
Method for measuring materials associated with huperzine A orally disintegrating tablets by high performance liquid chromatography (HPLC) Download PDFInfo
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- CN102043024A CN102043024A CN2009102361747A CN200910236174A CN102043024A CN 102043024 A CN102043024 A CN 102043024A CN 2009102361747 A CN2009102361747 A CN 2009102361747A CN 200910236174 A CN200910236174 A CN 200910236174A CN 102043024 A CN102043024 A CN 102043024A
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- huperzine
- oral cavity
- water
- disintegration tablet
- cavity disintegration
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Abstract
The invention discloses a HPLC measurement method for materials associated with huperzine A orally disintegrating tablets. In the method, a chromatographic column taking octadecylsilane chemically bonded silica as a filler is adopted, and mixed solvent of acetonitrile serving as an organic phase and a water phase is used as a flowing phase. The method can be used for controlling the quality of the huperzine A orally disintegrating tablets.
Description
Technical field:
The present invention relates to a kind of high performance liquid chromatogram method, particularly a kind of high-performance liquid chromatogram determination method of huperzine-A oral cavity disintegration tablet related substance.
Background technology:
Huperzine is the reversibility anticholinesterase, has the effect that promotes that memory represents and enhance memory keep, and can improve senile memory function and go down.Molecular formula is C
15H
18N
2O, chemical being called (5R, 9R, 11E)-and 5-amino-11-ethidine-5,6,9,10-tetrahydrochysene-7-methyl-5,9-methylene ring suffering is (B) pyridine-2 (1H) ketone also, and its structural formula is as follows:
This law adopts common chromatographic column (C
18Chromatographic column) realizes the mensuration of huperzine-A oral cavity disintegration tablet related substance fast and accurately, thereby realized the control of each impurity of huperzine-A oral cavity disintegration tablet, guaranteed the quality controllable of huperzine-A oral cavity disintegration tablet, had realistic meaning.
Summary of the invention:
The object of the present invention is to provide a kind of method, can be used for the quality control of huperzine-A oral cavity disintegration tablet with high efficiency liquid chromatography for separating and determining huperzine-A oral cavity disintegration tablet related substance.
The invention provides a kind of method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance, selecting octadecylsilane chemically bonded silica for use is the chromatographic column of filler, and the mixed solvent that with the acetonitrile is organic phase and water is as moving phase.
The invention provides a kind of method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance, is the mixed solvent of organic phase and water in the moving phase, and organic phase and water ratio are 1: 5～5: 9.
The invention provides a kind of method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance, moving phase is the mixed solvent of organic phase and water, and organic phase and water ratio are 1: 9.
The invention provides a kind of method with high performance liquid chromatography survey huperzine-A oral cavity disintegration tablet related substance, described water is a phosphate buffer, and its pH scope is 2～5.
The invention provides a kind of method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance, described phosphate is selected from a kind of or its potpourri in sodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, sodium pentanesulfonate or the sodium heptanesulfonate.
The invention provides a kind of method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance, described phosphate is potassium dihydrogen phosphate.
The invention provides a kind of method, can realize by the following method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance:
It is an amount of to get the huperzine-A oral cavity disintegration tablet fine powder, with the moving phase dissolving, is mixed with the sample solution that every 1ml contains huperzine 0.5mg, detects wavelength 310nm, selects C for use
18Chromatographic column, 25 ℃ of column temperatures.Extracting sample solution 20 μ l inject high performance liquid chromatograph, finish the mensuration of huperzine-A oral cavity disintegration tablet related substance.
1) it is an amount of to get the huperzine-A oral cavity disintegration tablet fine powder, uses the moving phase sample dissolution, and is mixed with the sample solution that every 1ml contains huperzine 0.5mg.
2) flow rate of mobile phase being set is 0.5～1.5ml/min, and the flow velocity of moving phase is preferably 1.0ml/min; Detect wavelength 210～320nm, the optimum detection wavelength is 310nm; Select C for use
18Chromatographic column; 20～30 ℃ of chromatographic column column temperatures, column temperature the best are 25 ℃.
3) get 1) sample solution 10～50 μ l, preferred 20 μ l inject high performance liquid chromatograph, finish the mensuration of huperzine-A oral cavity disintegration tablet related substance.
The present invention can effectively measure the related substance of huperzine-A oral cavity disintegration tablet, the method simple and fast, and the sensitivity for analysis height, the result is accurately and reliably.The quality control of available huperzine-A oral cavity disintegration tablet.
Description of drawings
The oxidation of Fig. 1 huperzine destroys the high-efficient liquid phase chromatogram of sample
The oxidation of Fig. 2 huperzine-A oral cavity disintegration tablet destroys the high-efficient liquid phase chromatogram of sample
The blank auxiliary material oxidation of Fig. 3 huperzine-A oral cavity disintegration tablet destroys the high-efficient liquid phase chromatogram of sample
The high-efficient liquid phase chromatogram of the blank auxiliary material of Fig. 4 huperzine-A oral cavity disintegration tablet
The high-efficient liquid phase chromatogram of Fig. 5 huperzine-A oral cavity disintegration tablet
Embodiment:
Following examples are used for further understanding the present invention, but are not limited to the scope of this enforcement.
Embodiment 1
Instrument and condition
Day island proper Tianjin LC-10ATVP pump, Tianjin, island SPD-10AVP ultraviolet-visible light multiwavelength detector, RHEODYNE 7725i injector and TL9900 chromatographic data workstation, chromatographic column: Apollo-C
18250 * 4.6mm, 5 μ m, ultraviolet detection wavelength: 310nm, moving phase: acetonitrile-pH2.5 phosphate buffered solution (get potassium dihydrogen phosphate 2.72g, the water dissolved dilution is to 1000ml, and transferring pH with 10% phosphoric acid,diluted is 2.5 ± 0.05) (10: 90).
Experimental procedure
Get the about 12mg of huperzine, place the 25ml measuring bottle, oxidation destroyed after 3 days in 30% hydrogen peroxide, added the moving phase dissolving and was diluted to scale, shook up, as need testing solution I.Get huperzine-A oral cavity disintegration tablet fine powder and blank auxiliary material fine powder an amount of (being equivalent to huperzine 5mg approximately) in addition respectively, place the 10ml measuring bottle, oxidation destroyed after 3 days in 30% hydrogen peroxide, it is an amount of to add moving phase, the ultrasonic huperzine that makes dissolves, and is diluted to scale with moving phase, shakes up, filter, subsequent filtrate is respectively as need testing solution II and need testing solution III.
Get need testing solution I, II, III, carry out high-efficient liquid phase analysis according to above-mentioned condition, the record chromatogram the results are shown in Fig. 1～3 respectively.
Retention time is that 13.569 minutes chromatographic peak is the chromatographic peak of huperzine among Fig. 1, and Fig. 2 retention time is that 13.877 minutes chromatographic peak is the chromatographic peak of huperzine.Fig. 3 can show that there is tangible chromatographic peak in relative main peak retention time in the auxiliary material blank on less than 0.25 position, and Fig. 1 shows and do not occur the impurity that destroys out in the position that blank auxiliary material goes out the peak, so should give deduction during calculating.Fig. 1～3 show that each impurity of huperzine-A oral cavity disintegration tablet separates with main peak well, and blank auxiliary material detects noiseless to impurity, and this law can be used for the quality monitoring of huperzine-A oral cavity disintegration tablet.
Instrument and condition
Day island proper Tianjin LC-10ATVP pump, Tianjin, island SPD-10AVP ultraviolet-visible light multiwavelength detector, RHEODYNE 7725i injector and TL9900 chromatographic data workstation, chromatographic column: Apollo-C
18250 * 4.6mm, 5 μ m, ultraviolet detection wavelength: 310nm, moving phase: acetonitrile-pH2.5 phosphate buffered solution (get potassium dihydrogen phosphate 2.72g, the water dissolved dilution is to 1000ml, and transferring pH with 10% phosphoric acid,diluted is 2.5 ± 0.05) (10: 90).
Experimental procedure
Get huperzine-A oral cavity disintegration tablet fine powder an amount of (being equivalent to huperzine 5mg approximately), place the 10ml measuring bottle, it is an amount of to add moving phase, and the ultrasonic huperzine that makes dissolves, and is diluted to scale with moving phase, shakes up, and filters, and subsequent filtrate is as need testing solution.Get need testing solution, carry out high-efficient liquid phase analysis according to above-mentioned condition, and carry out the auxiliary material blank test, the results are shown in Figure 4, Fig. 5 with method.
Fig. 4 proves, there is tangible chromatographic peak in main peak retention time relatively in the auxiliary material blank on less than 0.25 position, is deducted during calculating; Retention time is that 12.841 minutes chromatographic peak is the chromatographic peak of huperzine among Fig. 5, the single impurity of its related substance is less than 2.0%, total impurities is less than 4.0%, the result shows that the related substance of huperzine-A oral cavity disintegration tablet reaches the requirement of preparation, and this law can be used for the quality monitoring of huperzine Pharmaceutical composition.
Claims (7)
1. method with high-performance liquid chromatogram determination huperzine-A oral cavity disintegration tablet related substance, it is characterized in that selecting for use octadecylsilane chemically bonded silica is the chromatographic column of filler, the mixed solvent that with the acetonitrile is organic phase and water is as moving phase.
2. method according to claim 1, its feature moving phase are to be the mixed solvent of organic phase and water with the acetonitrile, and the ratio of organic phase and water is 1: 5～5: 9.
3. method according to claim 2, its feature moving phase are to be the mixed solvent of organic phase and water with the acetonitrile, and the ratio of organic phase and water is 1: 9.
4. according to each described method of claim 1～3, it is characterized in that described water is a phosphate buffer, its pH scope is 2～5.
5. method according to claim 4 is characterized in that described phosphate is selected from a kind of or its potpourri in sodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, sodium pentanesulfonate or the sodium heptanesulfonate.
6. method according to claim 5 is characterized in that described phosphate is potassium dihydrogen phosphate.
7. according to each described method of claim 1～6, it is characterized in that: it is an amount of to get the huperzine-A oral cavity disintegration tablet fine powder, with the moving phase dissolving, is mixed with the sample solution that every 1ml contains huperzine 0.5mg, detects wavelength 310nm, selects C for use
18Chromatographic column, 25 ℃ of column temperatures, extracting sample solution 20 μ l inject high performance liquid chromatograph, finish the mensuration of huperzine-A oral cavity disintegration tablet related substance.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016054286A1 (en) * | 2014-10-03 | 2016-04-07 | Amphastar Pharmaceuticals, Inc. | Methods of resolving racemic mixture to obtain (-)-huperzine a |
| CN109613156A (en) * | 2018-09-06 | 2019-04-12 | 万邦德制药集团股份有限公司 | A kind of huperzine and detection method of the huperzine injection in relation to substance |
-
2009
- 2009-10-22 CN CN2009102361747A patent/CN102043024A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 国家药典委员会: "《中国药典2005版第二部》", 31 December 2005 * |
| 谢元超 等: "替代对照品法用于石杉碱甲片含量测定的研究", 《中国药学杂志》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016054286A1 (en) * | 2014-10-03 | 2016-04-07 | Amphastar Pharmaceuticals, Inc. | Methods of resolving racemic mixture to obtain (-)-huperzine a |
| US10287249B2 (en) | 2014-10-03 | 2019-05-14 | Amphastar Pharmaceuticals, Inc. | Methods of resolving racemic mixture to obtain (−)-huperzine A |
| US10829455B2 (en) | 2014-10-03 | 2020-11-10 | Amphastar Nanjing Pharmaceuticals Inc. | Methods of resolving racemic mixture to obtain (−)-Huperzine A |
| CN109613156A (en) * | 2018-09-06 | 2019-04-12 | 万邦德制药集团股份有限公司 | A kind of huperzine and detection method of the huperzine injection in relation to substance |
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Application publication date: 20110504 |