CN108845065A - Measure the HPLC method in relation to substance in sulphadiazine suspension - Google Patents
Measure the HPLC method in relation to substance in sulphadiazine suspension Download PDFInfo
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- CN108845065A CN108845065A CN201810632358.4A CN201810632358A CN108845065A CN 108845065 A CN108845065 A CN 108845065A CN 201810632358 A CN201810632358 A CN 201810632358A CN 108845065 A CN108845065 A CN 108845065A
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- sulphadiazine
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention discloses the HPLC methods in relation to substance in a kind of measurement sulphadiazine suspension, and -0.3% ammonium acetate of acetonitrile is used to carry out gradient elution for mobile phase；Reference substance is dissolved using -0.3% ammonium acetate of mobile phase acetonitrile, sample, which is taken, is first added after quantitative sodium hydroxide test solution dissolution again plus flows phase dilution.Studies have shown that sulphadiazine concentration linear relationship is good using mobile phase and type of elution of the invention, a large amount of impurity peaks can be detected, and impurity peaks can be efficiently separated with main peak, impurity mean sample recovery rate is high；Meanwhile the preparation of solution directlys adopt mobile phase to dissolve reference substance, sample, which is taken, to be first added after quantitative sodium hydroxide test solution dissolution again plus flows phase dilution, and method is easy to operate, and can be to avoid the influence of solvent.As it can be seen that specificity of the present invention is strong, accuracy is high, and reproducibility is good, can be used for the quality control of sulphadiazine suspension.
Description
Technical field
The invention belongs to sulphadiazine suspension technical field of quality detection more particularly to a kind of measurement sulphadiazine to be suspended
HPLC method in liquid in relation to substance.
Background technique
Sulfa drugs (Sulfonamides, SAs) is a kind of antibacterials, and has a broad antifungal spectrum, absorption is rapider, can be pressed down
Most of gram-positive bacterias and certain Gram-negative bacterias are made, and have inhibiting effect to a small number of fungies, protozoon and virus, are commonly used
To treat the infection of the upper respiratory tract, enteric infection, skin pyogenic infection and tonsillitis etc..Sulphadiazine (sulfadiazine)
It is a kind of sulfa drugs that application is wider, it is mainly used for preventing and treating bacterium sense as a kind of chemical antibacterial-anti-inflammatory drug
Infectious diseases.Sulphadiazine suspension is the suspension aqueous solution of sulphadiazine fine particle, fine precipitate after standing, after shaking at
Uniform white suspension is clinically mainly used for the infection such as hemolytic streptococcus, meningococcus, pneumococcus.
Sulphadiazine bulk pharmaceutical chemicals are recorded in Chinese Pharmacopoeia (ChP 2015), British Pharmacopoeia (BP2017), United States Pharmacopeia
(USP40), European Pharmacopoeia (EP9.0) has Related substances separation item in addition to Chinese Pharmacopoeia.Sulphadiazine suspension only records
Chinese Pharmacopoeia version (ChP 2015) in 2015, but without Related substances separation item.Current medical safety issue has become full society
Meeting increasingly focus of attention, and the research of related substance and control are one of the key element that drug safety guarantees, various countries' drug
Requirement of the quality standard to Related substances separation is also higher and higher.Related substances separation research is in current China's drug research and development
One of weak spot.Want the safety of horizontal, practical guarantee public's medication of General Promotion China drug research and development, it is necessary to pay attention to and add
Strong related object Quality Research.
Summary of the invention
The technical problem to be solved in the present invention is to provide it is a kind of it is easy to operate, specificity is strong, accuracy is high, reproducibility is good
Measurement sulphadiazine suspension in the HPLC method in relation to substance, for use in sulphadiazine suspension quality control.
In order to solve the above technical problems, the present invention uses following technical scheme：
The HPLC method in relation to substance in sulphadiazine suspension is measured, uses -0.3% ammonium acetate of acetonitrile for mobile phase progress
Gradient elution；Reference substance is dissolved using -0.3% ammonium acetate of mobile phase acetonitrile, sample, which is taken, is first added quantitative sodium hydroxide
Add flowing phase dilution after test solution dissolution again.
Chromatographic condition is：Shiseido Capcell PAK MGIIC18 chromatographic column (4.6mm × 250mm, 5 μm), with 0.3%
Ammonium acetate solution is mobile phase A, and acetonitrile is Mobile phase B, carries out gradient elution, flow velocity：1.0mL·min-1, Detection wavelength：
260nm, column temperature：30 DEG C, sample volume：10μl.
Gradient elution is carried out by following procedure：
。
Operation is carried out as follows in the preparation of solution：
<1>Reference substance stock solution：Respectively precision weigh sulphadiazine reference substance 51.86mg, impurity A reference substance 50.76mg,
Impurity B reference substance 42.14mg, impurity C reference substance 51.11mg, impurity D reference substance 51.07mg, set in same 100ml measuring bottle, add
Sodium hydroxide test solution 1ml makes to dissolve, and is diluted to scale with mobile phase, shake up to get；Impurity A is 2- aminopyrimidine, impurity B
For p-aminobenzene sulfonic acid, impurity C is sulphoamidine, and impurity D is sulfanilamide (SN)；
<2>Reference substance uses liquid：Precision measures mixing reference substance stock solution 3ml, sets in 100ml measuring bottle, adds mobile phase dilute
Release to scale, shake up to get；
<3>Test solution：Precision measures sulphadiazine suspension 5ml, sets in 100ml measuring bottle, adding sodium hydroxide test solution
5ml makes to dissolve, and mobile phase is added to be diluted to scale, shakes up, and filters, and precision measures subsequent filtrate 5ml, sets in 50ml measuring bottle, with stream
Phase dilution is moved to scale, is shaken up, as test solution；
<4>Own control solution：Precision measures test solution 0.1ml, sets in 100ml measuring bottle, mobile phase is added to be diluted to
Scale shakes up, and takes subsequent filtrate as own control solution.
<5>Sodium hydroxide test solution：Take sodium hydroxide 4.3g, be dissolved in water into 100ml to get.
Aiming at the problem that sulphadiazine suspension lacks related substance detection, it is phonetic that inventor establishes a kind of measurement sulfanilamide (SN)
HPLC method in pyridine suspension in relation to substance uses -0.3% ammonium acetate of acetonitrile to carry out gradient elution for mobile phase；Using flowing
- 0.3% ammonium acetate of phase acetonitrile dissolves reference substance, and sample, which is taken, to be first added after quantitative sodium hydroxide test solution dissolution again plus flowing
Phase dilution.Studies have shown that sulphadiazine concentration linear relationship is good using mobile phase and type of elution of the invention, can detect
A large amount of impurity peaks out, and impurity peaks can be efficiently separated with main peak, impurity mean sample recovery rate is high；Meanwhile solution
Preparation directly adopt mobile phase to dissolve reference substance, sample, which is taken, to be first added after quantitative sodium hydroxide test solution dissolution again plus stream
Dynamic phase dilution, method is easy to operate, and can be to avoid the influence of solvent.As it can be seen that specificity of the present invention is strong, accuracy is high, reappears
Property it is good, can be used for sulphadiazine suspension quality control.
Detailed description of the invention
Fig. 1 is HPLC chromatogram of the present invention, in figure：A：Sample, B：Acid destroys, C：Alkali destroys, D：Oxidative demage, E：Illumination
It destroys, F：High temperature；2. impurity B；4. impurity C；7. impurity A；8. impurity D；11. sulphadiazine.
Specific embodiment
One, instrument and reagent
1.1 instrument
Waters e2695 type high performance liquid chromatograph (band column oven and autosampler), the inspection of 2998 type diode arrays
Survey device (200nm~400nm full wavelength scanner) and Empower chromatographic work station (Waters, US)；XD205DU electronics day
Flat (Mettler Toledo Inc. of Switzerland)；The desk-top baking oven of ED53 BINDER；(University Of Tianjin is accurate for YB-2 type clarity detecting apparatus
Instrument plant)；Milli-Q A10 pure water generator.
1.2 reagent
Sulphadiazine reference substance (National Institute for Food and Drugs Control, lot number：100026-201404, content 99.7%)；
Impurity A reference substance (2- aminopyrimidine, Stanford Analytical Chemicals Inc, lot number：AL170221-13；Contain
Amount is 100%)；Impurity B reference substance (p-aminobenzene sulfonic acid, Nat'l Pharmaceutical & Biological Products Control Institute, lot number：101180-201001,
Content 100%)；Impurity C reference substance (sulphoamidine, National Institute for Food and Drugs Control, lot number：100412-201302, content
92.0%)；Impurity D reference substance (sulfanilamide (SN), National Institute for Food and Drugs Control, lot number：100024-201103, content
99.8%)；Sulphadiazine suspension (producer A, sample lot number：170206,170511,170708；10%) specification is；Water is super
Pure water, acetonitrile are chromatographically pure, other reagents are that analysis is pure.
Two, method and result
2.1 chromatographic condition
Chromatographic column：Shiseido Capcell PAK MG II C18 chromatographic column (4.6mm × 250mm, 5 μm), with 0.3% second
Acid ammonium solution is mobile phase A, and acetonitrile is Mobile phase B, carries out gradient elution, flow velocity by table 1：1.0mL·min-1, Detection wavelength：
260nm, column temperature：30 DEG C, sample volume：10μl.
1 gradient elution program of table
The preparation of 2.2 solution
2.2.1 precision weighs sulphadiazine reference substance 51.86mg, impurity A reference substance to reference substance stock solution respectively
50.76mg, impurity B reference substance 42.14mg, impurity C reference substance 51.11mg, impurity D reference substance 51.07mg, set same 100ml
In measuring bottle, adding sodium hydroxide test solution 1ml makes to dissolve, and is diluted to scale with mobile phase, and shaking up to get concentration is about 0.5mg/ml
Mixing reference substance stock solution.
2.2.2 reference substance measures mixing reference substance stock solution 3ml using liquid precision, sets in 100ml measuring bottle, adds mobile phase dilute
It releases to scale, shaking up to get concentration is about 15 μ gml-1Mixing reference substance use solution.
2.2.3 test solution precision measures sulphadiazine suspension 5ml, sets in 100ml measuring bottle, adding sodium hydroxide test solution
5ml makes to dissolve, and mobile phase is added to be diluted to scale, shakes up, and filters, and precision measures subsequent filtrate 5ml, sets in 50ml measuring bottle, with stream
Phase dilution is moved to scale, shakes up, as test solution, sees Figure 1A.
2.2.4 own control solution precision measures test solution 0.1ml, sets in 100ml measuring bottle, mobile phase is added to be diluted to
Scale shakes up, and takes subsequent filtrate as own control solution.
2.2.5 sodium hydroxide test solution takes sodium hydroxide 4.3g, be dissolved in water into 100ml to get.
The test of 2.3 specificities
2.3.1 acid destroys accurate measurement sulphadiazine suspension 0.5ml, adds hydrochloric acid lml, places 1 hour, adding sodium hydroxide
Test solution tune pH weakly acidic pH, adds mobile phase to be diluted to scale, shakes up, and filtering takes 10 μ l of subsequent filtrate, injects liquid chromatograph, record
Chromatogram is shown in Figure 1B.
2.3.2 alkali destroys accurate measurement sulphadiazine suspension 0.5ml, adding sodium hydroxide test solution 1ml, places 1 hour, adds
Hydrochloric acid tune pH weakly acidic pH adds mobile phase to be diluted to scale, shakes up, and filtering takes 10 μ l of subsequent filtrate, injects liquid chromatograph, records color
Spectrogram is shown in Fig. 1 C.
2.3.3 Oxidative demage precision measures sulphadiazine suspension 0.5ml, adds 30% hydrogen peroxide 1ml, places 1 hour,
It is diluted to scale with mobile phase, is shaken up, is filtered, 10 μ l of subsequent filtrate is taken, injects liquid chromatograph, chromatogram is recorded, sees Fig. 1 D.
2.3.4 illumination destroys accurate measurement sulphadiazine suspension 0.5ml, irradiates one week under 4500Lx illumination condition,
Add 5ml sodium hydroxide test solution to make to dissolve, be diluted to scale with mobile phase, shake up, filter, take 10 μ l of subsequent filtrate, injects liquid phase color
Spectrometer records chromatogram, sees Fig. 1 E.
2.3.5 high temperature precision measures sulphadiazine suspension 0.5ml, places 5h in 105 DEG C of baking ovens, adds 5ml hydrogen-oxygen
Changing sodium test solution makes to dissolve, and is diluted to scale with mobile phase, shakes up, and filters, and takes 10 μ l of subsequent filtrate, injects liquid chromatograph, record
Chromatogram is shown in Fig. 1 F.
Specificity test result shows and (is shown in Table 2), and sulphadiazine suspension is under acid, alkali, oxidation, illumination and hot conditions
There is apparent catabolite to generate, related content of material increases.Each catabolite and principal component peak can reach good point
From, show the chromatographic condition be able to satisfy this product related substance detection.
2 sample of table and strong destruction test result
2.4 ranges of linearity and detection limit, quantitative limit measurement
Precision measure " 2.2.2 " item under mixing reference substance using each 0.1ml, 0.5ml of liquid, 1.0ml, 5.0ml,
10.0ml is respectively placed in 10ml measuring bottle, then be further diluted to scale with mobile phase, and being prepared into concentration is about 0.15 μ g
ml-1、0.75μg·ml-1、1.5μg·ml-1、7.5μg·ml-1、15μg·ml-1Series standard solution, by under " 2.1 " item
Chromatographic condition measurement, records chromatogram, and using concentration as abscissa, peak area is that ordinate carries out linear regression analysis.By curve 1
The signal-to-noise ratio that solution obtains calculates separately the concentration of each reference substance solution as signal-to-noise ratio S/N=3 and S/N=10 as detection
Limit and quantitative limit, the results are shown in Table 3.
3 regression equation of table, related coefficient, the range of linearity, detection limit and quantitative limit
2.5 repetitive test
Sample (lot number 170206) is taken to prepare 6 parts of test solution by the method under " 2.2.3 " item, by under " 2.1 " item
Chromatographic condition be measured, calculate content by Standard reference, impurity C in sample, impurity D average content be respectively
0.010%, 0.073%；RSD is respectively 1.0%, 0.8%.The result shows that this method repeatability is good.
2.6 precision test
Take mixing reference substance under " 2.2.2 " item using liquid, be measured by the chromatographic condition under " 2.1 " item, continuously into
Sample 6 times, the RSD of each Component peak area is calculated, the RSD at each peak is respectively less than 1.0%, the results showed that the precision of instrument is good.
The test of 2.7 sample recovery rates
It is accurate respectively to measure totally 9 parts of 5ml sulphadiazine suspension, it respectively sets in 100ml measuring bottle, adding sodium hydroxide test solution 5ml
Make after dissolution accurate impurity reference substance stock solution 2.4ml, 3.0ml and 3.6ml being added under " 2.2.1 " item respectively again, each 3
Part, then it is diluted to scale with mobile phase, and it shakes up, filters, it is accurate respectively to measure 5ml, it respectively sets in 50ml measuring bottle, adds flowing phase dilution
To scale, shake up to get the rate of recovery solution of basic, normal, high concentration (80%, 100% and 120%).By the condition under " 2.1 " item
Measurement, calculate impurity A, impurity B, impurity C, impurity D average recovery rate be respectively 101.2%, 99.9%, 100.8% and
103.7%, RSD are respectively 1.6%, 0.8%, 0.8% and 0.6%.
2.8 stability test
Precision measures sulphadiazine suspension 5ml, sets in 100ml measuring bottle, and adding sodium hydroxide test solution 5ml makes to dissolve, accurate
The impurity reference substance stock solution 3ml under " 2.2.1 " item is added, is diluted to scale with mobile phase, shakes up, filters, precision measures continuous
Filtrate 5ml is set in 50ml measuring bottle, is diluted to scale with mobile phase.In at room temperature place 0,2,4,6,8,12,18, for 24 hours after, press
Chromatographic condition under " 2.1 " item is measured, and records each Component peak area, calculates sulphadiazine and impurity A, B, C, D peak area
RSD, as a result respectively 0.3%, 1.5%, 0.7%, 0.8%, 0.7%.The result shows that test solution is placed at room temperature for for 24 hours surely
It is fixed.
2.9 Related substances separation
Take sulphadiazine suspension (the sample lot number of three batches：170206, " 2.2.3 " item 170511,170708), is pressed
Under method prepare test solution, be measured by above-mentioned chromatographic condition, the results are shown in Table 4.
Table 4 is in relation to substance-measuring result
Sulphadiazine raw material standard regulation impurity A, B limit must not cross 0.3% in British Pharmacopoeia (BP2017), other are single
Maximum contaminant content must not cross 0.05%, and total impurities must not cross 0.5%.With this limit to the related object of sulphadiazine suspension
Matter is determined, the results showed that, the related substance of three batch samples meets regulation, and impurity A, B are not detected in sample.
Three, it discusses
The selection of 3.1 mobile phases
The method that inventor records referring to European Pharmacopoeia 9.0 uses acetonitrile -2.8g/L phosphoric acid (10；90) it is used as mobile phase,
The related substance for carrying out isocratic elution measurement sulphadiazine suspension, as a result, it has been found that with this condition, impurity 1,3 peaks are not protected
It stays, the mobile phase is not applicable.It uses -0.3% ammonium acetate of acetonitrile for mobile phase, carries out gradient elution, can detect a large amount of miscellaneous
Mass peak, and impurity peaks can be efficiently separated with main peak.
The selection of 3.2 wavelength
It is found by DAD full wavelength scanner, the maximum of a length of 260nm of the maximum absorption wave of sulphadiazine, impurity A, B, C, D
Absorbing wavelength is respectively 224nm, 249nm, 260nm, 258nm.Absorption value of the impurity A at 260nm is lower, but comprehensively considers logical
Cross the impurity higher in 260nm response, and detecting at this wavelength of impurity 1,3,10,14,15 of failure test generation
Quantity is most, and peak area is maximum, and final choice 260nm is as measurement wavelength.
3.3 durability
Use the chromatographic column of 3 brands：CAPCELL PAK MG II C18(4.6mm × 250mm, 5 μm), Agilent 5
HC-C18(2) (250 × 4.6mm, 5 μm), Yi Lite Hypersil ODS2C18Column (4.6mm × 250mm, 4 μm), it is same again respectively
Durability investigation is carried out on one high performance liquid chromatograph, as a result peak shape and separating effect difference are little, this law good tolerance.
3.4 brief summary
This research is measured the related substance in sulphadiazine suspension using HPLC gradient elution method, as a result shows
Show, the sulphadiazine suspension of three batches of different lot numbers meets the bound requirements in British Pharmacopoeia (BP2017).This method operation
Simply, easy, good separating effect, high sensitivity can be used as detection method of the sulphadiazine suspension in relation to substance, be into one
Step improves drug standard and provides foundation.
Claims (4)
1. the HPLC method in relation to substance in a kind of measurement sulphadiazine suspension, it is characterised in that：Using -0.3% acetic acid of acetonitrile
Ammonium is that mobile phase carries out gradient elution；Reference substance is dissolved using -0.3% ammonium acetate of mobile phase acetonitrile, sample, which is taken, to be first added
Add flowing phase dilution again after quantitative sodium hydroxide test solution dissolution.
2. the HPLC method in relation to substance in measurement sulphadiazine suspension according to claim 1, it is characterised in that chromatography
Condition is：Shiseido Capcell PAK MGIIC18 chromatographic column, using 0.3% ammonium acetate solution as mobile phase A, acetonitrile is flowing
Phase B carries out gradient elution, flow velocity：1.0mL·min-1, Detection wavelength：260nm, column temperature：30 DEG C, sample volume：10μl.
3. the HPLC method in relation to substance in measurement sulphadiazine suspension according to claim 1, it is characterised in that：It is described
Gradient elution is carried out by following procedure：
。
4. the HPLC method in relation to substance in measurement sulphadiazine suspension according to claim 1, it is characterised in that solution
Preparation operation is carried out as follows：
<1>Reference substance stock solution：Precision weighs sulphadiazine reference substance 51.86mg, impurity A reference substance 50.76mg, impurity respectively
B reference substance 42.14mg, impurity C reference substance 51.11mg, impurity D reference substance 51.07mg, set in same 100ml measuring bottle, add hydrogen-oxygen
Changing sodium test solution 1ml makes to dissolve, and is diluted to scale with mobile phase, shake up to get；The impurity A is 2- aminopyrimidine, impurity B
For p-aminobenzene sulfonic acid, impurity C is sulphoamidine, and impurity D is sulfanilamide (SN)；
<2>Reference substance uses liquid：Precision measures mixing reference substance stock solution 3ml, sets in 100ml measuring bottle, mobile phase is added to be diluted to
Scale, shake up to get；
<3>Test solution：Precision measures sulphadiazine suspension 5ml, sets in 100ml measuring bottle, adding sodium hydroxide test solution 5ml makes
Dissolution, and mobile phase is added to be diluted to scale, it shakes up, filters, precision measures subsequent filtrate 5ml, sets in 50ml measuring bottle, dilute with mobile phase
It releases to scale, shakes up, as test solution；
<4>Own control solution：Precision measures test solution 0.1ml, sets in 100ml measuring bottle, mobile phase is added to be diluted to scale,
It shakes up, takes subsequent filtrate as own control solution.
<5>Sodium hydroxide test solution：Take sodium hydroxide 4.3g, be dissolved in water into 100ml to get.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114778711A (en) * | 2022-03-14 | 2022-07-22 | 江苏金申医药科技有限公司 | Method for analyzing related substances of sulfadoxine |
| CN115097026A (en) * | 2022-06-08 | 2022-09-23 | 河北常山生化药业股份有限公司 | Method for detecting pyrazolopyrimidine benzene sulfonate compound from medicine |
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| EP0069097A2 (en) * | 1981-06-18 | 1983-01-05 | Astra Läkemedel Aktiebolag | Pharmaceutical mixture |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114778711A (en) * | 2022-03-14 | 2022-07-22 | 江苏金申医药科技有限公司 | Method for analyzing related substances of sulfadoxine |
| CN115097026A (en) * | 2022-06-08 | 2022-09-23 | 河北常山生化药业股份有限公司 | Method for detecting pyrazolopyrimidine benzene sulfonate compound from medicine |
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| CN108845065B (en) | 2021-06-22 |
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Effective date of registration: 20220127 Address after: 546100 standard workshops 11 and 16, No. 419 Shengtang Road (high tech Industrial Development Zone), overseas Chinese District, Laibin City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Minglei Weisheng Pharmaceutical Co.,Ltd. Address before: No.9, Qinghu Road, Qingxiu District, Nanning City, Guangxi Zhuang Autonomous Region Patentee before: GUANGXI INSTITUTE FOR FOOD AND DRUG CONTROL |