CN101825613A - Method for determining related substance of compound paracetamol and tramadol hydrochloride tablet through high-performance liquid chromatography - Google Patents
Method for determining related substance of compound paracetamol and tramadol hydrochloride tablet through high-performance liquid chromatography Download PDFInfo
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- CN101825613A CN101825613A CN200910079129A CN200910079129A CN101825613A CN 101825613 A CN101825613 A CN 101825613A CN 200910079129 A CN200910079129 A CN 200910079129A CN 200910079129 A CN200910079129 A CN 200910079129A CN 101825613 A CN101825613 A CN 101825613A
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Abstract
The invention discloses a method for determining related substances of a compound paracetamol and tramadol hydrochloride tablet through high-performance liquid chromatography. In the method, octyl silane bonded silica is used as a packing chromatographic column, and a mixed solvent with methanol as an organic phase and a water phase is used as a mobile phase. The method can be used for quality control of paracetamol and tramadol hydrochloride tablets and other types of compound drugs containing acetaminophen and tramadol hydrochloride.
Description
Technical field:
The present invention relates to the high-performance liquid chromatogram determination method of a kind of efficient liquid-phase chromatography method, particularly a kind of related substance of compound paracetamol and tramadol hydrochloride tablet through.
Background technology:
Paracetamol and tramadol hydrochloride tablet is an analgesic, is used for the treatment of because of the Acute Pain of spraining, pulling, arthritis ache outbreak, postoperative pain, wound, fracture etc. causing.
Paracetamol and tramadol hydrochloride tablet is the compound preparation of paracetamol and tramadol hydrochloride, and preparation intermediate product and final products are carried out quality control, guarantees that security of products, validity and reliability are very important.
This law adopts common C8 chromatographic column to realize the rapid and accurate determination of paracetamol and tramadol hydrochloride tablet related substance, thereby realized the quality control of the intermediate product and the finished product of paracetamol and tramadol hydrochloride tablet, guarantee the security and the reliability of paracetamol and tramadol hydrochloride 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 preparation process of paracetamol and tramadol hydrochloride tablet and the quality control of final products with the high efficiency liquid chromatography for separating and determining related substance of compound paracetamol and tramadol hydrochloride tablet through.
The invention provides a kind of method with the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through, selecting octyl silane key and silica gel for use is the chromatographic column of filler, and the mixed solvent that with methyl alcohol is organic phase and water is as moving phase.
The invention provides a kind of method with the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through, the organic phase in the moving phase is a methyl alcohol, and the ratio of methyl alcohol and water is: 20～50: 80～50.
The invention provides a kind of method with the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through, the organic phase in the moving phase is a methyl alcohol, and the ratio of methyl alcohol and water is: 30: 70.
The invention provides a kind of method with the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through, described water is a phosphate buffer, and its pH scope is 3～8.
The invention provides a kind of method with the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through, 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 the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through, described phosphate is potassium dihydrogen phosphate.
The invention provides a kind of method, can realize by the following method with the high-performance liquid chromatogram determination related substance of compound paracetamol and tramadol hydrochloride tablet through:
It is an amount of to get the paracetamol and tramadol hydrochloride tablet fine powder, and water dissolves, and is mixed with the sample solution of the many 4.0mg of every 1ml saliferous love song horse, and flow velocity is 1ml/min, detects wavelength 270nm, selects the C8 chromatographic column for use, 25 ℃ of column temperatures.Extracting sample solution 10ul injects high performance liquid chromatograph, finishes the mensuration of paracetamol and tramadol hydrochloride tablet related substance.
It is an amount of to get the paracetamol and tramadol hydrochloride tablet fine powder, the water dissolving, be mixed with every 1ml and contain the sample solution of paracetamol 0.5mg approximately, flow velocity is 1ml/min, detects wavelength 241nm, selects the C8 chromatographic column for use, 25 ℃ of column temperatures, extracting sample solution 10ul injects high performance liquid chromatograph, finishes the mensuration of paracetamol related substance in the paracetamol and tramadol hydrochloride tablet.
1) gets an amount of water sample dissolution of paracetamol and tramadol hydrochloride tablet sample, and be mixed with the sample solution of the many 4.0mg of the about saliferous love song of every 1ml horse, paracetamol 0.5mg respectively.
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, tramadol hydrochloride optimum detection wavelength is 270nm, paracetamol optimum detection wavelength 241nm; Select the C8 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 10ul injects high performance liquid chromatograph respectively, finishes the mensuration of paracetamol and tramadol hydrochloride tablet related substance.
The present invention can effectively measure the related substance of the bent horse multi-disc of compound paracetamol, 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 paracetamol, tramadol hydrochloride.
Description of drawings
The high-efficient liquid phase chromatogram of Fig. 1 paracetamol and tramadol hydrochloride tablet (blank auxiliary material)
The high-efficient liquid phase chromatogram of Fig. 2 paracetamol and tramadol hydrochloride tablet tramadol hydrochloride related substance
The high-efficient liquid phase chromatogram of Fig. 3 paracetamol and tramadol hydrochloride tablet paracetamol related substance
The high-efficient liquid phase chromatogram of Fig. 4 tramado hydrochloride dispersing tablet (blank auxiliary material)
The high-efficient liquid phase chromatogram of Fig. 5 tramado hydrochloride dispersing tablet tramadol hydrochloride related substance
The high-efficient liquid phase chromatogram of Fig. 6 tramado hydrochloride dispersing tablet paracetamol related substance
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: C8250 * 4.6mm, 5 μ m, the tramadol hydrochloride related substance detects wavelength: 270nm, the paracetamol related substance detects wavelength: 241nm, moving phase: phosphate buffer (is got potassium dihydrogen phosphate 6.80g, triethylamine 7.0ml, be dissolved in water and be diluted to 1000ml, transferring pH with 10% phosphoric acid,diluted is 5.0)-methyl alcohol (70: 30)
Experimental procedure
Get paracetamol and tramadol hydrochloride tablet fine powder an amount of (being equivalent to tramadol hydrochloride 40mg approximately), place the 10ml measuring bottle, the water dissolving also is diluted to scale, and is ultrasonic, filters, and gets subsequent filtrate as need testing solution.
Get paracetamol and tramadol hydrochloride tablet fine powder an amount of (being equivalent to paracetamol 5.0mg approximately), place the 10ml measuring bottle, the water dissolving also is diluted to scale, and is ultrasonic, filters, and gets 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. 3.
Fig. 1 proves that blank auxiliary material is the disturbed specimen determination of related substances not.Retention time is that 15.761 minutes chromatographic peak is the many chromatographic peaks of bent horse among Fig. 2, and retention time is that 6.200 minutes chromatographic peak is the chromatographic peak of paracetamol among Fig. 3, and remaining chromatographic peak is the chromatographic peak of sample impurity.The single impurity of tramadol hydrochloride related substance is less than 0.5%, and total impurities is less than 1.0%, and the single impurity of paracetamol related substance is less than 0.5%, and total impurities is less than 1.0%.The result shows that the related substance of paracetamol and tramadol hydrochloride tablet reaches the preparation requirement, and this law can be used for the quality monitoring of paracetamol and tramadol hydrochloride tablet.
Blank under these conditions auxiliary material does not disturb the chromatographic peak of tramadol hydrochloride and paracetamol and impurity to detect, and the requirement of Chinese Pharmacopoeia is satisfied in the test of chromatographic condition system suitability.
Embodiment 2
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: C8 250 * 4.6mm, 5 μ m, the tramadol hydrochloride related substance detects wavelength: 270nm, the paracetamol related substance detects wavelength: 241nm, moving phase: phosphate buffer (is got potassium dihydrogen phosphate 6.80g, triethylamine 7.0ml, be dissolved in water and be diluted to 1000ml, transferring pH with 10% phosphoric acid,diluted is 5.0)-methyl alcohol (70: 30)
Experimental procedure
Get tramado hydrochloride dispersing tablet fine powder an amount of (being equivalent to tramadol hydrochloride 40mg approximately), place the 10ml measuring bottle, the water dissolving also is diluted to scale, and is ultrasonic, filters, and gets subsequent filtrate as need testing solution.
Get tramado hydrochloride dispersing tablet fine powder an amount of (being equivalent to paracetamol 5.0mg approximately), place the 10ml measuring bottle, the water dissolving also is diluted to scale, and is ultrasonic, filters, and gets 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 4, Fig. 5, Fig. 6.
Fig. 4 proves that blank auxiliary material is the disturbed specimen determination of related substances not.Retention time is that 14.887 minutes chromatographic peak is the many chromatographic peaks of bent horse among Fig. 5, retention time is that 7.044 minutes chromatographic peak is the chromatographic peak of paracetamol among Fig. 6, wherein the single impurity of tramadol hydrochloride related substance is less than 0.5%, total impurities is less than 1.0%, the single impurity of paracetamol related substance is less than 0.5%, total impurities is less than 1.0%, the result shows that the related substance of tramado hydrochloride dispersing tablet reaches the preparation requirement, and this law can be used for the quality monitoring of tramado hydrochloride dispersing tablet.
Blank under these conditions auxiliary material does not disturb the chromatographic peak of tramadol hydrochloride and paracetamol 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 high-performance liquid chromatogram determination paracetamol and tramadol hydrochloride tablet related substance, it is characterized in that selecting for use octyl silane group silica gel is the chromatographic column of filler, the mixed solvent that with methyl alcohol 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 a methyl alcohol, and the ratio of methyl alcohol 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 a methyl alcohol, and the ratio of methyl alcohol 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 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 paracetamol and tramadol hydrochloride tablet fine powder, water dissolves, and is mixed with the sample solution of the many 4.0mg of every 1ml about saliferous love song horse, and flow velocity is 1ml/min, detect wavelength 270nm, select the C8 chromatographic column for use, 25 ℃ of column temperatures, extracting sample solution 10ul, inject high performance liquid chromatograph, finish the mensuration of tramadol hydrochloride related substance in the paracetamol and tramadol hydrochloride tablet; It is an amount of to get the paracetamol and tramadol hydrochloride tablet fine powder, the water dissolving, be mixed with every 1ml and contain the sample solution of paracetamol 0.5mg approximately, flow velocity is 1ml/min, detects wavelength 241nm, selects the C8 chromatographic column for use, 25 ℃ of column temperatures, extracting sample solution 10ul injects high performance liquid chromatograph, finishes the mensuration of paracetamol related substance in the paracetamol and tramadol hydrochloride tablet.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106353428A (en) * | 2016-09-19 | 2017-01-25 | 山西好医生药业有限公司 | Quality standard for paracetamol and tramadol hydrochloride capsules |
| CN106525994A (en) * | 2016-09-19 | 2017-03-22 | 山西好医生药业有限公司 | Method for determination of related substances of paracetamol and tramadol hydrochloride capsules |
| CN110501441A (en) * | 2019-09-27 | 2019-11-26 | 地奥集团成都药业股份有限公司 | Detection method in relation to substance in a kind of paracetamol tablets |
| CN111751470A (en) * | 2020-07-07 | 2020-10-09 | 多多药业有限公司 | Detection control method for new impurities in tramadol hydrochloride preparation and impurities obtained by detection control method |
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| DE2308079A1 (en) * | 1973-02-19 | 1974-08-22 | Volkswagenwerk Ag | ELASTIC UNIT SUSPENSION |
| CN101025409A (en) * | 2006-02-23 | 2007-08-29 | 信谊药厂 | Method for determining impurities for paracetamol and tramadol hydrochloride preparation |
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- 2009-03-04 CN CN200910079129A patent/CN101825613A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2308079A1 (en) * | 1973-02-19 | 1974-08-22 | Volkswagenwerk Ag | ELASTIC UNIT SUSPENSION |
| CN101025409A (en) * | 2006-02-23 | 2007-08-29 | 信谊药厂 | Method for determining impurities for paracetamol and tramadol hydrochloride preparation |
Non-Patent Citations (4)
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| CECCATO A 等: "Automated determination of tramadol enantiomers in human plasma using solid-phase extraction in combination with chiral liquid chromatography", 《JOURNAL OF CHROMATOGRAPHY B》 * |
| 刘晓红等: "HPLC法同时测定曲马氨酚片中盐酸曲马多和对乙酰氨基酚的含量", 《沈阳药科大学学报》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106353428A (en) * | 2016-09-19 | 2017-01-25 | 山西好医生药业有限公司 | Quality standard for paracetamol and tramadol hydrochloride capsules |
| CN106525994A (en) * | 2016-09-19 | 2017-03-22 | 山西好医生药业有限公司 | Method for determination of related substances of paracetamol and tramadol hydrochloride capsules |
| CN106525994B (en) * | 2016-09-19 | 2020-05-22 | 山西好医生药业有限公司 | Method for determining related substances of paracetamol and tramadol capsule |
| CN106353428B (en) * | 2016-09-19 | 2020-08-25 | 山西好医生药业有限公司 | Quality standard of paracetamol and tramadol capsule |
| CN110501441A (en) * | 2019-09-27 | 2019-11-26 | 地奥集团成都药业股份有限公司 | Detection method in relation to substance in a kind of paracetamol tablets |
| CN110501441B (en) * | 2019-09-27 | 2021-11-26 | 地奥集团成都药业股份有限公司 | Method for detecting related substances in acetaminophen tablet |
| CN111751470A (en) * | 2020-07-07 | 2020-10-09 | 多多药业有限公司 | Detection control method for new impurities in tramadol hydrochloride preparation and impurities obtained by detection control method |
| CN111751470B (en) * | 2020-07-07 | 2023-05-05 | 多多药业有限公司 | Detection control method for new impurities in tramadol hydrochloride preparation |
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Application publication date: 20100908 |