CN1793904B - Method of simultanaously detecting racemic methylephedrine hydrochloride, hydrobromic acid youmeishafen and clofenetamine maleate composition - Google Patents
Method of simultanaously detecting racemic methylephedrine hydrochloride, hydrobromic acid youmeishafen and clofenetamine maleate composition Download PDFInfo
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- CN1793904B CN1793904B CN 200510097030 CN200510097030A CN1793904B CN 1793904 B CN1793904 B CN 1793904B CN 200510097030 CN200510097030 CN 200510097030 CN 200510097030 A CN200510097030 A CN 200510097030A CN 1793904 B CN1793904 B CN 1793904B
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Abstract
A method for simultaneously detecting compositions of despun methylphedrine hydrochloride, hydrobromic acid dexmethaphen and maleic acid chlorpheniramine in compound includes applying high efficient liquid-phase chromatography; using octadecyl silane linkage silica gel as filler; using mixed solvent of methanol, acetonitrile, water and tetrahydrofuran as mobile phase; adding sulfosodium auccinatedicaprylate; using acid to regulate pH value; feeding in sample once to detect three compositions simultaneously.
Description
Technical field
The present invention a kind ofly can detect three kinds of main active racemization mephedrines, dextromethorphan hydrobromide and chlorphenamine maleate method for compositions contained in the Coritab simultaneously, and concrete is to adopt high performance liquid chromatography to composition discriminating, content and method for determination related substances.
Background technology
Flu is a kind of respiratory system common disease, frequently-occurring disease, clinical manifestation with headache, nasal obstruction, runny nose, feel sick, heating is cardinal symptom.Cold drug of the present invention is a compound preparation, contain the racemization mephedrine, dextromethorphan hydrobromide and chlorphenamine maleate the active base composition, also contain paracetamol, vitamin C, be used for antipyretic-antalgic, antibechic, alleviate runny nose, nasal obstruction, symptoms such as sneeze, bad reaction is few, safe, chlorphenamine maleate wherein is an antihistaminic, dextromethorphan hydrobromide is a non-narcotic maincenter antitussive, it is fine that effect is breathed heavily in the cough-relieving of racemization mephedrine, there is not the central nervous excitation effect, habituation hardly, almost non-toxic spinoff, and present state contains the list of mephedrine, compound preparation seldom, this compound preparation can effectively be alleviated the various symptoms that cause because of flu.
Because racemization mephedrine, dextromethorphan hydrobromide and chlorphenamine maleate are the main ingredient composition in this compound preparation, need accurately to measure the content of three kinds of compositions when this product quality of control, the method that adopts has volumetric analysis, ultraviolet spectrophotometry and high performance liquid chromatography at present.Assay all adopts volumetric analysis in racemization mephedrine (JP13) drug standards and the dextromethorphan hydrobromide drug standards, " 2005 editions two chlorphenamine maleate contents of Chinese pharmacopoeia are measured and are adopted volumetric analysis, the Chlorate assay adopts ultraviolet spectrophotometry, and volumetric analysis must extract each component drug respectively in the compound preparation from preparation, measure each components contents respectively with the method for volumetry titration again, the method complexity, complex operation, time-consuming, precision, accuracy and reappearance are all relatively poor, measure nearly week age once consuming time, poor practicability.Ultraviolet spectrophotometry is measured each components contents respectively, and sample pre-treatments bothers very much, and reappearance is also relatively poor; Have not yet to see high performance liquid chromatography determines three kinds of medicament contgs simultaneously under same chromatographic condition the method for using, and need adopt different moving phase and different column temperature conditions, when switching different condition determinations, equilibration time is oversize, is not suitable for drug quality control.
Summary of the invention
The objective of the invention is at above the deficiencies in the prior art, study that a kind of method is simple, accuracy is high, favorable reproducibility can detect racemization mephedrine, dextromethorphan hydrobromide and chlorphenamine maleate method for compositions simultaneously, and can be used as discriminating, content and the method for determination related substances of these three kinds of compositions.
The object of the invention can be achieved through the following technical solutions:
The present invention realizes with efficient liquid-phase chromatography method, may further comprise the steps:
1. stationary phase is an octadecylsilane chemically bonded silica;
2. the ratio of moving phase alcohol, acetonitrile, water, tetrahydrofuran mixed solvent is (150-200): (400-450): (300-400): (30-70), preferred proportion is (160-190): (400-430): (320-380): (40-60), alcoholic solvent can be methyl alcohol or ethanol;
3. the addition of dioctylis sulfosuccinas natricus in moving phase is 0.1%-1.0%, and preferred amounts is 0.35%-0.5%;
4. regulating the used acid of moving phase pH value can be phosphoric acid or acetic acid; Moving phase pH value scope 4.5-5.5;
5. used UV-detector is in wavelength 258 ± 2nm place inspection side;
6. flow rate of mobile phase 0.5-1.5ml/min;
7. sample dissolves with moving phase, sample size 20 μ l;
8. the detection limit of three components is respectively racemization mephedrine 50ng, dextromethorphan hydrobromide 20ng, chlorphenamine maleate 0.4ng.
Mixed solvent of the present invention also can obtain good separation detection effect with alcohol, acetonitrile, water, tetrahydrofuran, and the mixed solvent component as hereinbefore.
Mixed solvent of the present invention also can obtain good separation detection effect with methyl alcohol or ethanol, acetonitrile, water, tetrahydrofuran, and the mixed solvent component as hereinbefore.
The technology of the present invention progress is that method is simple, and is highly sensitive, and method is single-minded.Adopt the present invention can once measure racemization mephedrine, dextromethorphan hydrobromide and content for Chlorphenamine Maleate and related substance simultaneously.Sample only needs to get final product direct injected after the filtration with the moving phase dissolving, measures and once is no more than 30 minutes.This method precision height, good stability, other compositions of sample and auxiliary material do not influence mensuration, and the recovery of high, medium and low concentration is all better, and reappearance is better, and method is easy and simple to handle, and is reliable and stable, practical, is fit to very much controllable quality.
Description of drawings
Fig. 1 is the chromatogram of one of testing sample of the present invention.
Embodiment
Further explain the present invention with embodiment below, but protection scope of the present invention is not limited to embodiment.
Embodiment one
With octadecylsilane chemically bonded silica is filling agent; (180: 420: 350: 50), adding dioctylis sulfosuccinas natricus 4.45g among every 1000ml, was moving phase with phosphorus acid for adjusting pH value to 5.0, and the detection wavelength is 258nm with methyl alcohol-acetonitrile-water-tetrahydrofuran.Getting this product 15 grams (containing racemization mephedrine 50mg, dextromethorphan hydrobromide 40mg, chlorphenamine maleate 6.25mg approximately) puts in the 250ml measuring bottle, add the moving phase ultrasonic dissolution, put and be chilled to room temperature, be diluted to scale with moving phase, shake up, filter, precision is measured subsequent filtrate 20 μ l, inject liquid chromatograph, the record chromatogram; Precision takes by weighing chlorphenamine maleate reference substance 12.5mg in addition, puts in the measuring bottle of 50ml, adds the moving phase dissolving and is diluted to scale, as chlorphenamine maleate reference substance stock solution; Mephedrine reference substance 20mg, dextromethorphan hydrobromide reference substance 16mg are revolved in cancellation, the accurate title, decide, put in the same 100ml measuring bottle, the accurate chlorphenamine maleate reference substance stock solution 10ml that adds, add the moving phase dissolving and be diluted to scale, shake up, measure with method, press external standard method with calculated by peak area, promptly.Chromatogram is seen Fig. 1 (retention time of racemization mephedrine, chlorphenamine maleate and dextromethorphan hydrobromide is respectively 8.353min, 15.233min, 18.698min).
Embodiment two
With octadecylsilane chemically bonded silica is filling agent; (150: 450: 370: 30), adding dioctylis sulfosuccinas natricus 5.0g among every 1000ml, was moving phase with vinegar acid for adjusting pH value to 5.0, and the detection wavelength is 258nm with ethanol-acetonitrile-water-tetrahydrofuran.Getting this product 15 grams (containing racemization mephedrine 50mg, dextromethorphan hydrobromide 40mg, chlorphenamine maleate 6.25mg approximately) puts in the 250ml measuring bottle, add the moving phase ultrasonic dissolution, put and be chilled to room temperature, be diluted to scale with moving phase, shake up, filter, precision is measured subsequent filtrate 20 μ l, inject liquid chromatograph, the record chromatogram; Precision takes by weighing chlorphenamine maleate reference substance 12.5mg in addition, puts in the measuring bottle of 50ml, adds the moving phase dissolving and is diluted to scale, as chlorphenamine maleate reference substance stock solution; Mephedrine reference substance 20mg, dextromethorphan hydrobromide reference substance 16mg are revolved in cancellation, the accurate title, decide, put in the same 100ml measuring bottle, the accurate chlorphenamine maleate reference substance stock solution 10ml that adds, add the moving phase dissolving and be diluted to scale, shake up, measure with method, press external standard method with calculated by peak area, promptly.
Embodiment three
With octadecylsilane chemically bonded silica is filling agent; (200: 400: 330: 70), adding dioctylis sulfosuccinas natricus 3.5g among every 1000ml, was moving phase with phosphorus acid for adjusting pH value to 5.0, and the detection wavelength is 258nm with methyl alcohol-acetonitrile-water-tetrahydrofuran.Getting this product 15 grams (containing racemization mephedrine 50mg, dextromethorphan hydrobromide 40mg, chlorphenamine maleate 6.25mg approximately) puts in the 250ml measuring bottle, add the moving phase ultrasonic dissolution, put and be chilled to room temperature, be diluted to scale with moving phase, shake up, filter, precision is measured subsequent filtrate 20 μ l, inject liquid chromatograph, the record chromatogram; Precision takes by weighing chlorphenamine maleate reference substance 12.5mg in addition, puts in the measuring bottle of 50ml, adds the moving phase dissolving and is diluted to scale, as chlorphenamine maleate reference substance stock solution; Mephedrine reference substance 20mg, dextromethorphan hydrobromide reference substance 16mg are revolved in cancellation, the accurate title, decide, put in the same 100ml measuring bottle, the accurate chlorphenamine maleate reference substance stock solution 10ml that adds, add the moving phase dissolving and be diluted to scale, shake up, measure with method, press external standard method with calculated by peak area, promptly.
Claims (8)
1. a detection simultaneously contains active ingredient racemization mephedrine, dextromethorphan hydrobromide and chlorphenamine maleate method for compositions, adopt high performance liquid chromatography, it is characterized in that: with octadecylsilane chemically bonded silica is filling agent, with moving phase alcohol, acetonitrile, water, tetrahydrofuran mixed solvent is moving phase, and the adding dioctylis sulfosuccinas natricus, regulate moving phase pH value with acid, sample dissolves with moving phase, flow velocity 0.5-1.5ml/min detects wavelength 258 ± 2nm; Moving phase alcohol is methyl alcohol or ethanol.
2. method according to claim 1 is characterized in that: the ratio of moving phase alcohol, acetonitrile, water, tetrahydrofuran mixed solvent is (150-200): (400-450): (300-400): (30-70).
3. method according to claim 2 is characterized in that: the ratio of moving phase alcohol, acetonitrile, water, tetrahydrofuran mixed solvent is (160-190): (400-430): (320-380): (40-60).
4. method according to claim 2 is characterized in that, the ratio of mobile phase methanol, acetonitrile, water, tetrahydrofuran mixed solvent is 180: 420: 350: 50.
5. method according to claim 1 is characterized in that: the addition of dioctylis sulfosuccinas natricus in moving phase is 0.1%-1.0%g/ml.
6. method according to claim 6 is characterized in that: the addition of dioctylis sulfosuccinas natricus in moving phase is 0.35%-0.5%g/ml.
7. method according to claim 1 is characterized in that: regulating the used acid of moving phase pH value can be phosphoric acid or acetic acid.
8. method according to claim 1 is characterized in that: moving phase pH value scope 4.5-5.5.
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| CN 200510097030 CN1793904B (en) | 2005-12-30 | 2005-12-30 | Method of simultanaously detecting racemic methylephedrine hydrochloride, hydrobromic acid youmeishafen and clofenetamine maleate composition |
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| CN 200510097030 CN1793904B (en) | 2005-12-30 | 2005-12-30 | Method of simultanaously detecting racemic methylephedrine hydrochloride, hydrobromic acid youmeishafen and clofenetamine maleate composition |
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| CN1793904B true CN1793904B (en) | 2011-02-16 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273361A (en) * | 2000-06-08 | 2000-11-15 | 复旦大学 | Method for detecting composition of carena, methoxyphenamine hydrochloride, narcotine, etc at same time |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273361A (en) * | 2000-06-08 | 2000-11-15 | 复旦大学 | Method for detecting composition of carena, methoxyphenamine hydrochloride, narcotine, etc at same time |
Non-Patent Citations (4)
| Title |
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| 吴俊文 等.反相高效液相色谱法测定复方美沙芬糖浆主料含量.山西医科大学学报35 4.2004,35(4),379-380页. |
| 吴俊文等.反相高效液相色谱法测定复方美沙芬糖浆主料含量.山西医科大学学报35 4.2004,35(4),379-380页. * |
| 姜红 等.高效液相色谱法测定酚麻美敏片的含量.中国现代应用药学杂志16 3.1999,16(3),全文，尤其第3小节. |
| 姜红等.高效液相色谱法测定酚麻美敏片的含量.中国现代应用药学杂志16 3.1999,16(3),全文,尤其第3小节. * |
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