CN103353486A - High performance liquid chromatography method for determining content of quinine sulfate in quinine sulfate tablet - Google Patents
High performance liquid chromatography method for determining content of quinine sulfate in quinine sulfate tablet Download PDFInfo
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- CN103353486A CN103353486A CN2013102381450A CN201310238145A CN103353486A CN 103353486 A CN103353486 A CN 103353486A CN 2013102381450 A CN2013102381450 A CN 2013102381450A CN 201310238145 A CN201310238145 A CN 201310238145A CN 103353486 A CN103353486 A CN 103353486A
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- quinine sulfate
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- phosphoric acid
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Abstract
The invention discloses a high performance liquid chromatography method for determining the content of quinine sulfate in a quinine sulfate tablet. For the chromatographic conditions, a reversed-phase chromatographic column with octadecyl silane as the filler is selected as the chromatographic column. The mobile phase consists of acetonitrile and a phosphate buffer solution (prepared by dissolving 6.8g of potassium dihydrogen phosphate in 1000ml of water, and adjusting the pH to 4 with phosphoric acid) in a ratio of 10:90, the flow rate is 1.0ml/min, the column temperature is 35DEG C, and the detection wavelength is 250nm. The result shows that: quinine sulfate has a good linear relationship (R2=1) with the peak area in a concentration range of 0.4mg/ml-2.0mg/ml, the average sample recovery rate is 101.99%, and RSD=2.8% (n=3). The method has the advantages of simple operation, accurate result, reliability, and good repeatability.
Description
Technical field
The present invention relates to the Pharmaceutical Analysis field, a kind of high performance liquid chromatography of measuring quinine sulfate content in the quinine sulfate sheet of specific requirement protection.
Background technology
Quinine sulfate is quinoline derivatives (structure is seen accompanying drawing 1), can be combined with plasmodial DNA, form compound and suppress copying of DNA and transcribing of RNA, thereby the albumen that suppresses protozoon is synthetic, a little less than effect than chloroquine is.Be applicable to the malignant malaria due to chloroquine and the strain of anti-multi-medicament worm.
The quinine sulfate sheet disc-shaped preparation that to be quinine sulfate form with compacting after the auxiliary material such as starch evenly mixes has sugar-coat to be coated with outward.2010 editions content control methods about the quinine sulfate sheet of Chinese Pharmacopoeia are the perchloric acid titration method, this method temperature influence is larger, and the titration end-point change color is affected by human factors larger by artificial judgement, the different operating person operates the larger error of existence, and the testing result reappearance is low.The invention discloses quinine sulfate content in a kind of high effective liquid chromatography for measuring quinine sulfate sheet, simple to operate, precision is high, and favorable reproducibility has important practical value for the quality control of quinine sulfate sheet.
Summary of the invention
The present invention seeks to set up the method for quinine sulfate tablet quality control, the content of quinine sulfate uses high performance liquid chromatography to measure and control in the quinine sulfate sheet.Concrete by following technical method enforcement:
Chromatographic condition:
It is the reverse-phase chromatographic column of filling agent that chromatographic column is selected octadecyl silane.
Mobile phase is the mixed solution of phosphate buffer and acetonitrile.Quinine sulfate is quinoline derivatives, and mobile phase adds the composition of phosphate buffer, can improve detection sensitivity, and the quinine sulfate solution ph is in 5.7～6.6 scopes, and mobile phase is transferred about PH to 4.0 with phosphoric acid solution, the wash-out that is easy to quinine sulfate with separate.Wherein the phosphoric acid buffer liquid making method is: take by weighing the 6.8g potassium dihydrogen phosphate, with the water-soluble solution of 1000ml, phosphoric acid is transferred PH to 4.0.
During acetonitrile and phosphate buffer ratio optimization are tested in the mobile phase, the acetonitrile volume ratio is 10%～45%, wherein preferred 10%, when the acetonitrile volume ratio is 45%～15%, do not meet the standard of Chinese Pharmacopoeia degree of separation separating than all less than 1.5 of main peak and impurity peaks, and the acetonitrile volume ratio is 10%, main peak and impurity peaks degree of separation are 6.15, and main peak and impurity separating effect are fine.
Detecting device uses the DAD detecting device, determines that quinine sulfate has preferably uv absorption at 190nm～260nm, and maximum absorption wavelength is 250nm, and the related substances of quinine sulfate also has preferably absorption under this wavelength, detects the preferred 250nm of wavelength.The quinine sulfate ultraviolet absorpting spectrum is seen accompanying drawing 2.
Flow velocity is 1ml/min, sampling volume 5 μ l.
Solution preparation:
The quinine sulfate standard solution: the accurately weighed 20～50mg standard items of difference, place the 25ml volumetric flask, add the ultrasonic 15min of a certain amount of mobile phase with sample dissolution, be settled to scale mark with mobile phase again.
Quinine sulfate sheet solution: get this product, remove dressing, porphyrize, accurately weighed an amount of (being equivalent to approximately quinine sulfate 40mg), and place the 25ml volumetric flask, add the ultrasonic 15min of a certain amount of mobile phase with sample dissolution, be settled to scale mark with mobile phase again.
Quantitative analysis method:
The present invention demarcates quinine sulfate content in the quinine sulfate sheet with external standard method, in 0.4mg/ml～2mg/ml scope, select respectively 5 sample concentrations to formulate calibration curve, need testing solution gained peak area substitution calibration curve calculates, and namely gets quinine sulfate content in the need testing solution.
Description of drawings
Fig. 1 is the quinine sulfate structural formula.
Fig. 2 is the quinine sulfate ultraviolet absorpting spectrum.
Fig. 3 is the collection of illustrative plates under the quinine sulfate 250nm wavelength.
Fig. 4 is the quinine sulfate typical curve.
Embodiment
Embodiment 1
Reagent and sample: chromatogram acetonitrile (Merck), potassium dihydrogen phosphate (AR), phosphoric acid (AR), ultrapure water, the long-range quinine sulfate sheet (the accurate word H42021750 of traditional Chinese medicines) of purchasing in Wuhan.
Instrument and equipment: Agilent-1260 high performance liquid chromatograph, Shanghai sound man of virtue and ability digital supersonic cleaning apparatus, 0.2 μ m organic system filtration unit, 0.45 μ m filter etc.
Chromatographic condition: mobile phase: acetonitrile: phosphate buffer (10: 90), wherein the phosphoric acid buffer liquid making method is: take by weighing the 6.8g potassium dihydrogen phosphate, with the water-soluble solution of 1000ml, phosphoric acid is transferred PH to 4.0.Mobile phase filters 2 times through 0.2 μ m filtrator, uses behind the ultrasonic degas 15min.
Solution preparation: the quinine sulfate standard solution-accurately weighed 9.8mg of difference, 21.3mg, 31.6mg, 41.3mg, 50.6mg standard items place respectively the 25ml volumetric flask, add the ultrasonic 15min of a certain amount of mobile phase with sample dissolution, be settled to scale mark with mobile phase again, be mixed with the standard solution of quinine sulfate.Quinine sulfate sheet solution-get this product is removed dressing, porphyrize, accurately weighed an amount of (being equivalent to approximately quinine sulfate 40mg), and place the 25ml volumetric flask, add the ultrasonic 15min of a certain amount of mobile phase with sample dissolution, be settled to scale mark with mobile phase again.
Quantitative analysis method: with standard solution and the need testing solution of preparation, difference injection liquid chromatography, gained standard items peak area is depicted as calibration curve, the substitution of need testing solution peak area is calculated, recording the long-range quinine sulfate sheet average content of purchasing for 3 times is 98.36%, the RSD value is 1.0%, and measurement result is reliable and stable.
Embodiment 2
1) precision is investigated: repeat to survey same standard items (selecting concentration is the 0.4mg/ml standard items) by the inventive method, the results are shown in Table 1.
The same standard items of table 1 repeat 5 sample introduction peak area results
2) reappearance is investigated: survey same batch sample 3 times by the inventive method, the results are shown in Table 2.
Table 2. is measured content 3 times with a collection of test sample
3) Specification Curve of Increasing
The accurately weighed 9.8mg of difference, 21.3mg, 31.6mg, 41.3mg, the 50.6mg standard items place respectively the 25ml volumetric flask, add the ultrasonic 15min of a certain amount of mobile phase with sample dissolution, are settled to scale mark with mobile phase again, are mixed with the standard solution of quinine sulfate.By the inventive method chromatographic condition sample introduction, (wherein X is quinine sulfate standard items quality, and Y is quinine sulfate standard items peak areas, R to get quinine sulfate typical curve (seeing accompanying drawing 4): Y=117.03X-13.454
2=1)
4) average recovery test
Take by weighing respectively the quinine sulfate sheet of known content through the powder 35.0mg of porphyrize, 22.0mg, 11.3mg put the 25ml volumetric flask, add respectively 11.2mg, 19.6mg, 27.3mg quinine sulfate standard items, add mobile phase and be mixed with solution, measure according to the inventive method sample introduction, gained peak area substitution quinine sulfate typical curve calculates yield, recovery result such as table 3.
Table 3 quinine sulfate average recovery
Claims (5)
1. the method for quinine sulfate content in the high effective liquid chromatography for measuring quinine sulfate sheet, it is characterized in that: it is the reverse-phase chromatographic column of filling agent that chromatographic column is selected octadecyl silane; Mobile phase is acetonitrile: phosphate buffer=10: 90; Flow velocity 1.0ml/min; 35 ℃ of column temperatures; Detect wavelength 250nm.
2. the method for claim 1 is characterized in that the phosphoric acid buffer liquid making method is: take by weighing the 6.8g potassium dihydrogen phosphate, use the water-soluble solution of 1000ml, phosphoric acid accent PH to 4.0.
3. the method for claim 1 is characterized in that sample dissolution mobile phase ultrasonic dissolution (100HZ, about 15min).
4. the method for claim 1 is characterized in that sizing technique selects external standard method that quinine sulfate content in the quinine sulfate sheet is demarcated, and quinine sulfate is good linear relation (R with peak area in 0.4mg/ml～2.0mg/ml concentration range
2=1).
5. the method for claim 1 is characterized in that the average average recovery of quinine sulfate is 101.99%, RSD=2.8% (n=3).
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766140A (en) * | 2012-08-14 | 2012-11-07 | 玉溪市维和生物技术有限责任公司 | Process for separating and preparing quinine sulfate from peruvian bark |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766140A (en) * | 2012-08-14 | 2012-11-07 | 玉溪市维和生物技术有限责任公司 | Process for separating and preparing quinine sulfate from peruvian bark |
Non-Patent Citations (4)
| Title |
|---|
| P.C. KAYUMBA 等: "Quinine sulphate pellets for flexible pediatric drug dosing:Formulation development and evaluation of taste-masking efficiency using the electronic tongue", 《EUROPEAN JOURNAL OF PHARMACEUTICS AND BIOPHARMACEUTICS 》, vol. 66, no. 3, 30 June 2007 (2007-06-30), pages 460 - 465 * |
| RAJAA A. MIRGHANI 等: "Simultaneous determination of quinine and four metabolites in plasma and urine by high-performance liquid chromatography", 《JOURNAL OF CHROMATOGRAPHY B》, vol. 754, no. 1, 15 April 2001 (2001-04-15), pages 57 - 94, XP004231989, DOI: doi:10.1016/S0378-4347(00)00577-6 * |
| SONG-YUN LIU 等: "HPLC and GC±MS screening of Chinese proprietary medicine for undeclared therapeutic substances", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》, vol. 24, no. 56, 31 March 2001 (2001-03-31), pages 983 - 992 * |
| 马飞 等: "硫酸奎宁纯度的测定及其不确定度的评定", 《测量与设备》, no. 3, 26 June 2012 (2012-06-26), pages 35 - 36 * |
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Application publication date: 20131016 |