CN101609070A - A kind of method of measuring related substances of losastan potassium/hydrochlorothiazide tablets with HPLC - Google Patents
A kind of method of measuring related substances of losastan potassium/hydrochlorothiazide tablets with HPLC Download PDFInfo
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- CN101609070A CN101609070A CNA2008101150956A CN200810115095A CN101609070A CN 101609070 A CN101609070 A CN 101609070A CN A2008101150956 A CNA2008101150956 A CN A2008101150956A CN 200810115095 A CN200810115095 A CN 200810115095A CN 101609070 A CN101609070 A CN 101609070A
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- potassium
- losastan
- acetonitrile
- hydrochlorothiazide tablets
- phosphate
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Abstract
The invention discloses a kind of high-efficient liquid phase chromatogram process measuring method of related substances of losastan potassium/hydrochlorothiazide tablets, selecting octadecylsilane key and silica gel for use is the chromatographic column of filler, the mixed solvent that with the acetonitrile is organic phase and water is as moving phase, can be used for losastan potassium/hydrochlorothiazide tablets and contains the quality control of other formulation compound medicine of Losartan Potassium, Hydrochioro.
Description
Technical field:
The present invention relates to a kind of efficient liquid-phase chromatography method, particularly a kind of high-performance liquid chromatogram determination method of compound preparation related substances of losastan potassium/hydrochlorothiazide tablets.
Background technology:
Losastan potassium/hydrochlorothiazide tablets is a drug for hypertension, is used for the treatment of hypertension.
Losastan potassium/hydrochlorothiazide tablets is the compound preparation of Losartan Potassium and Hydrochioro, for the quality control of preparation intermediate product and final products, guarantees that security of products, validity and reliability are very important.
This law adopts common C18 chromatographic column to realize the rapid and accurate determination of related substances of losastan potassium/hydrochlorothiazide tablets, thereby realized quality control to the intermediate product and the finished product of losastan potassium/hydrochlorothiazide tablets, guarantee the security and the reliability of losastan potassium/hydrochlorothiazide tablets, 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 preparation process of losastan potassium/hydrochlorothiazide tablets and the quality control of final products with high efficiency liquid chromatography for separating and determining compound preparation related substances of losastan potassium/hydrochlorothiazide tablets.
The invention provides a kind of method with high-performance liquid chromatogram determination compound preparation related substances of losastan potassium/hydrochlorothiazide tablets, selecting octadecylsilane key and silica gel 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 compound preparation related substances of losastan potassium/hydrochlorothiazide tablets, the organic phase in the moving phase is an acetonitrile, and the ratio of acetonitrile and water is: 20～50: 80～50.
The invention provides a kind of method with high-performance liquid chromatogram determination compound preparation related substances of losastan potassium/hydrochlorothiazide tablets, the organic phase in the moving phase is an acetonitrile, and the ratio of acetonitrile and water is: 30: 70.
The invention provides a kind of method with high-performance liquid chromatogram determination compound preparation related substances of losastan potassium/hydrochlorothiazide tablets, described water is a phosphate buffer, and its pH scope is 3～8.
The invention provides a kind of method with high-performance liquid chromatogram determination compound preparation related substances of losastan potassium/hydrochlorothiazide tablets, described phosphate is selected from a kind of or its potpourri in sodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate or the potassium dihydrogen phosphate.
The invention provides a kind of method with high-performance liquid chromatogram determination compound preparation related substances of losastan potassium/hydrochlorothiazide tablets, described phosphate is sodium hydrogen phosphate.
The invention provides a kind of method, can realize by the following method with high-performance liquid chromatogram determination compound preparation related substances of losastan potassium/hydrochlorothiazide tablets:
It is an amount of to get the losastan potassium/hydrochlorothiazide tablets fine powder, with the moving phase dissolving, is mixed with the sample solution that every 1ml contains Losartan Potassium 1.0mg, and flow velocity is 1ml/min, detects wavelength 225nm, selects the C18 chromatographic column for use, 25 ℃ of column temperatures.Extracting sample solution 20ul injects high performance liquid chromatograph, finishes the mensuration of related substances of losastan potassium/hydrochlorothiazide tablets.
1) gets the losastan potassium/hydrochlorothiazide tablets sample and use the moving phase sample dissolution in right amount, and be mixed with the sample solution that every 1ml contains Losartan Potassium 1.0mg approximately.
2) flow rate of mobile phase being set is 0.5～1.5ml/min, and the flow velocity of moving phase is preferably 1ml/min; Detect wavelength 210～280nm, the optimum detection wavelength is 225nm; Select the C18 chromatographic column for use; 20～30 ℃ of chromatographic column column temperatures, column temperature the best are 25 ℃.
3) get 1) sample solution 10～50ul, preferred 20ul injects high performance liquid chromatograph, finishes the mensuration of related substances of losastan potassium/hydrochlorothiazide tablets.
The present invention can effectively measure the related substance of compound preparation losastan potassium/hydrochlorothiazide tablets, and method is simple and efficient, the sensitivity for analysis height, and the result is accurately and reliably.Can be used for containing the quality control of the compound medicament composition of Losartan Potassium, Hydrochioro.
Description of drawings
The liquid chromatogram of Fig. 1 losastan potassium/hydrochlorothiazide tablets (blank auxiliary material)
The high-efficient liquid phase chromatogram of Fig. 2 losastan potassium/hydrochlorothiazide tablets
The high-efficient liquid phase chromatogram of Fig. 3 losartan potassium hydrochlorothiazide capsule (blank auxiliary material)
The high-efficient liquid phase chromatogram of Fig. 4 losartan potassium hydrochlorothiazide capsule
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 multiwavelength detector, RHEODYNE 7725i injector and TL9900 chromatographic data workstation, chromatographic column: C18 250 * 4.6mm, 5 μ m, ultraviolet detection wavelength: 225nm, moving phase: phosphate buffer (0.05mol/L disodium phosphate soln, transferring pH with 10% phosphoric acid,diluted is 6.5)-acetonitrile (70: 30)
Experimental procedure
Get losastan potassium/hydrochlorothiazide tablets fine powder an amount of (being equivalent to Losartan Potassium 10mg approximately), place the 10ml measuring bottle, add the moving phase dissolving and be diluted to scale, ultrasonic, filter, get subsequent filtrate as need testing solution.Other gets blank right amount of auxiliary materials, with the method operation, as blank auxiliary material solution.Get blank auxiliary material solution and need testing solution respectively, carry out high-efficient liquid phase analysis by above-mentioned condition, the record chromatogram the results are shown in Figure 1, Fig. 2.
Fig. 1 proves that blank auxiliary material is the disturbed specimen determination of related substances not.Retention time is that 2.283 minutes chromatographic peak is the chromatographic peak of Hydrochioro among Fig. 2, and retention time is that 11.117 minutes chromatographic peak is the chromatographic peak of Losartan Potassium, and remaining chromatographic peak is the chromatographic peak of sample impurity.The single impurity of Hydrochioro related substance is less than 0.5%, and total impurities is less than 1.0%, and the single impurity of Losartan Potassium related substance is less than 0.5%, and total impurities is less than 1.0%.The result shows that the related substance of losastan potassium/hydrochlorothiazide tablets reaches the preparation requirement, and this law can be used for the quality monitoring of losastan potassium/hydrochlorothiazide tablets.
Blank under these conditions auxiliary material does not disturb the chromatographic peak of Losartan Potassium and Hydrochioro and impurity to detect, and the requirement of Chinese Pharmacopoeia is satisfied in the test of chromatographic condition system suitability.
Instrument and condition
Day island proper Tianjin LC-10ATVP pump, Tianjin, island SPD-10AVP ultraviolet-visible multiwavelength detector, RHEODYNE 7725i injector and TL9900 chromatographic data workstation, chromatographic column: C18 250 * 4.6mm, 5 μ m, ultraviolet detection wavelength: 225nm, moving phase: phosphate buffer (0.05mol/L disodium phosphate soln, transferring pH with 10% phosphoric acid,diluted is 6.5)-acetonitrile (70: 30)
Experimental procedure
Get losartan potassium hydrochlorothiazide capsule particle fine powder an amount of (being equivalent to Losartan Potassium 10mg approximately), place the 10ml measuring bottle, add the moving phase dissolving and be diluted to scale, ultrasonic, filter, get subsequent filtrate as need testing solution.Other gets blank right amount of auxiliary materials, with the method operation, as blank auxiliary material solution.Get blank auxiliary material solution and need testing solution respectively, carry out high-efficient liquid phase analysis by above-mentioned condition, the record chromatogram the results are shown in Figure 3, Fig. 4.
Fig. 3 proves that blank auxiliary material is the disturbed specimen determination of related substances not.Retention time is that 5.683 minutes chromatographic peak is the chromatographic peak of Hydrochioro among Fig. 4, retention time is that 11.233 minutes chromatographic peak is the chromatographic peak of Losartan Potassium, wherein the single impurity of Hydrochioro related substance is less than 0.5%, total impurities is less than 1.0%, the single impurity of Losartan Potassium related substance is less than 0.5%, total impurities is less than 1.0%, and the result shows that the related substance of losartan potassium hydrochlorothiazide capsule reaches the preparation requirement, and this law can be used for the quality monitoring of Losartan Potassium.
Blank under these conditions auxiliary material does not disturb the chromatographic peak of Losartan Potassium and Hydrochioro and impurity to detect, and the requirement of Chinese Pharmacopoeia is satisfied in the test of chromatographic condition system suitability.
Claims (7)
1. method with the high-performance liquid chromatogram determination related substances of losastan potassium/hydrochlorothiazide tablets, it is characterized in that selecting for use octadecylsilane key and silica gel 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 is characterized in that the organic phase in the moving phase is an acetonitrile, and the ratio of acetonitrile and water is: 20～50: 80～50.
3. method according to claim 1 is characterized in that the organic phase in the moving phase is an acetonitrile, and the ratio of acetonitrile and water is: 30: 70.
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 3～8.
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 or the potassium dihydrogen phosphate.
6. method according to claim 5 is characterized in that described phosphate is sodium hydrogen phosphate.
7. according to each described method of claim 1～6, it is characterized in that: it is an amount of to get the losastan potassium/hydrochlorothiazide tablets fine powder, with the moving phase dissolving, be mixed with the sample solution that every 1ml contains Losartan Potassium 1.0mg approximately, flow velocity is 1ml/min, detect wavelength 225nm, select the C18 chromatographic column for use, 25 ℃ of column temperatures, extracting sample solution 10ul, inject high performance liquid chromatograph, finish the mensuration of related substances of losastan potassium/hydrochlorothiazide tablets.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101150956A CN101609070A (en) | 2008-06-16 | 2008-06-16 | A kind of method of measuring related substances of losastan potassium/hydrochlorothiazide tablets with HPLC |
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| CNA2008101150956A CN101609070A (en) | 2008-06-16 | 2008-06-16 | A kind of method of measuring related substances of losastan potassium/hydrochlorothiazide tablets with HPLC |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565221A (en) * | 2011-12-26 | 2012-07-11 | 浙江大学 | Method for measuring hydrochlorothiazide drug content by ion chromatography-ultraviolet detection method |
| CN102109501B (en) * | 2009-12-28 | 2013-07-17 | 扬子江药业集团上海海尼药业有限公司 | Method for detecting related substances in quinapril hydrochloride and hydrochlorothiazide composition |
| CN111220730A (en) * | 2020-01-19 | 2020-06-02 | 合肥科颖医药科技有限公司 | Analysis method of related substances in irbesartan and hydrochlorothiazide compound preparation |
| CN111443135A (en) * | 2020-01-10 | 2020-07-24 | 苏州国辰生物科技股份有限公司 | Method for determining concentrations of hydrochlorothiazide, losartan and losartan 5-carboxylate in plasma by liquid chromatography-mass spectrometry |
-
2008
- 2008-06-16 CN CNA2008101150956A patent/CN101609070A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102109501B (en) * | 2009-12-28 | 2013-07-17 | 扬子江药业集团上海海尼药业有限公司 | Method for detecting related substances in quinapril hydrochloride and hydrochlorothiazide composition |
| CN102565221A (en) * | 2011-12-26 | 2012-07-11 | 浙江大学 | Method for measuring hydrochlorothiazide drug content by ion chromatography-ultraviolet detection method |
| CN111443135A (en) * | 2020-01-10 | 2020-07-24 | 苏州国辰生物科技股份有限公司 | Method for determining concentrations of hydrochlorothiazide, losartan and losartan 5-carboxylate in plasma by liquid chromatography-mass spectrometry |
| CN111220730A (en) * | 2020-01-19 | 2020-06-02 | 合肥科颖医药科技有限公司 | Analysis method of related substances in irbesartan and hydrochlorothiazide compound preparation |
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Open date: 20091223 |