CN103353485A - High performance liquid chromatography for detecting quinine sulfate content - Google Patents
High performance liquid chromatography for detecting quinine sulfate content Download PDFInfo
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- CN103353485A CN103353485A CN2013102381446A CN201310238144A CN103353485A CN 103353485 A CN103353485 A CN 103353485A CN 2013102381446 A CN2013102381446 A CN 2013102381446A CN 201310238144 A CN201310238144 A CN 201310238144A CN 103353485 A CN103353485 A CN 103353485A
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Abstract
The invention relates to the drug content detection field, particularly to a high performance liquid chromatography for detecting a quinine sulfate content. And an external standard method is employed to determine the quinine sulfate content. The invention adopts a chromatographic condition of C18(4.6*250mm5micrometers), the mobile phase is composed of methanol and a 1% monopotassium phosphate solution in a ratio of 40:60, and phosphoric acid is taken to adjust the PH of the mobile phase to 4. An ultraviolet detector is used, and the detection wavelength is 316nm. The detection method provided in the invention has the advantages of: good linear relation between a sample concentration and a peak area, good separation effect, high accuracy, and simple and rapid analysis. The method determines that the linear range of quinine sulfate is 0.5 microgram/ml-100 microgram/ml, the linear correlation coefficient r is 1, and RDS is 0.59%.
Description
Technical field
The present invention relates to a kind of content assaying method of medicine, be specifically related to a kind of efficient liquid-phase chromatography method that detects quinine sulfate content.
Background technology
Quinine sulfate (structural formula is seen accompanying drawing 1) is the quinine Alkaloid, claims again quinine.Quinine sulfate chemical name: (8S, 9R)-6 '-methoxyl-quinine-9-alcohol radical sulfate dihydrate, molecular formula: (C
20H
24N
2O
2)
2H
2SO42H
2O, pure white needle-like is like crystallization, and is general matt.Be dissolved in hot water (1: 35) and ethanol (1: 125), be insoluble in chloroform and ether.Be exposed in the light dimmed brown.Odorless has lasting strong bitter taste.Quinine sulfate has the treatment malaria, the effects such as arrhythmia cordis and anti-inflammatory, and it 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.Be applicable to the malignant malaria due to chloroquine and the strain of anti-multi-medicament worm, also can be used for treating tertian fever.According to the up-to-date report of the World Health Organization (WHO), malaria is the infectious disease that obviously is in the world the trend of liter except acquired immune deficiency syndrome (AIDS), it is a kind of transmissible disease of subtropics and torrid areas, endangering the health of 2,000,000,000 populations, pernicious malaria causes people more than 400,000,000 to infect and 3,000,000 people death every year, has become the killer of harm humans health and lives in Africa.The report of studying in recent years quinine series of biologic alkali content is less, and the report of research quinine sulfate content still less.Open report: blue or green haze (fluorescence spectrophotometry quinine sulfate content, blue or green haze, Nanjing Medical University, 2012 years) report, utilize the quinine sulfate molecule to have the quinuclidine structure, can produce the characteristic of fluorescence, can directly use its fluorescence intensity of fluorescence spectrometry, obtain regression equation by calibration curve and obtain the concentration of quinine sulfate.The assay method of quinine sulfate content is adopted is the non-aqueous solution titrimetry for 2010 editions Chinese Pharmacopoeias in addition.Just measure at present in the method for quinine sulfate content, the testing result accuracy is low, and method of operating is loaded down with trivial details, and there is very large obstacle in accurate detection quinine sulfate content.In the detection method of the present invention, sample concentration and peak area linear relationship are good, good separating effect, and it is high to measure accuracy, analyzes the easy characteristics such as quick, has important using value for the content of quinine sulfate in Accurate Determining quinine sulfate preparation and the bulk drug.
Summary of the invention
The purpose of this invention is to provide that a kind of linear relationship is good, good separating effect, accuracy is high and analyze simple and rapid quinine sulfate detection method of content.For reaching above-mentioned purpose, the present invention has adopted following technical scheme:
In the specific embodiment of the present invention, the present invention adopts the content of high effective liquid chromatography for measuring quinine sulfate, namely adopts the content of external standard method quinine sulfate.
In another specific embodiment of the present invention, the present invention typical case but the liquid chromatograph of selecting that do not limit are: U.S. Agilent-1260 detects, UV-detector.
In another specific embodiment of the present invention, the present invention typical case but the selected chromatographic column that do not limit: C18 (4.6x250mm5 μ m).
In another specific embodiment of the present invention, it is 38-42: 62-58 that methyl alcohol that mobile phase is elected as and 1% potassium dihydrogen phosphate mix the volume ratio that forms, and it is 4 that phosphoric acid is transferred mobile phase PH, preferred 40: 60 of volume ratio.
The present invention advances in the specific embodiment, and described sample size is 1-20 μ l, preferred 5 μ l.
The present invention goes back in the specific embodiment, and the flow velocity of described mobile phase is 0.5-1.2mg/ml, preferred 1.0mg/ml.
Description of drawings
Fig. 1 is the quinine sulfate structural formula
Fig. 2 is quinine sulfate standard items liquid chromatograms
Fig. 3 is the quinine sulfate linear relationship
Fig. 4 is quinine sulfate standard items working curves
Embodiment
Chromatographic condition:
Adopt the Agilent-1260 high performance liquid chromatograph, with C18 reverse-phase chromatographic column C18 (4.6x250mm5 μ m);
Column temperature: 25 ℃.
Detecting device: UV-detector, detect wavelength 316nm.
Mobile phase solution: methyl alcohol-1% potassium dihydrogen phosphate=40: 60, it is 4 that phosphoric acid is transferred mobile phase PH.
Standard solution preparation: precision takes by weighing the 25.0mg standard items, places the 10ml volumetric flask, adds that mobile phase is ultrasonic to be made sample dissolution and be settled to scale mark.
Testing sample preparation: precision takes by weighing the testing sample with the standard items equivalent weight, places the 10ml volumetric flask, adds that mobile phase is ultrasonic to be made sample dissolution and be settled to scale mark.
According to the cubage formula:
Quinine sulfate content (%)=(A1XC2)/(A2XC1)
Wherein A1 is the testing sample peak area
A2 is the standard items peak area
C1 testing sample concentration (mg/ml)
C2 standard items concentration (mg/ml)
Bring data into and can obtain quinine sulfate content.
According to above-mentioned chromatographic condition, the content of demarcating that Malaysia is bought is that 98.0% quinine sulfate carries out assay.
Standard solution preparation: precision takes by weighing the 25.0mg standard items, places the 10ml volumetric flask, adds that mobile phase is ultrasonic to be made sample dissolution and be settled to scale mark.
Testing sample preparation: precision takes by weighing the Malay quinine sulfate sample of 25.0mg, places the 10ml volumetric flask, adds that mobile phase is ultrasonic to be made sample dissolution and be settled to scale mark.
Standard solution and testing sample are prepared 3 respectively, measure respectively 5 μ l and advance chromatographic column, and the gained peak area is averaged and brought above-mentioned formula calculating, result of calculation such as table 1 into.
Wherein, chromatographic column: C18 (4.6 * 250mm5 μ m); Mobile phase is methyl alcohol-1% potassium dihydrogen phosphate=40: 60, and it is 4 that phosphoric acid is transferred mobile phase PH; Chromatogram temperature: 25 ℃; Sample size: 5 μ l; Flow velocity: 1.0ml/min; Detecting device is UV-detector; Detect wavelength: 316nm.
The Malaysian sample determination result of table 1 such as following table
According to above-mentioned chromatographic condition, the content of demarcating that India is bought is that 99.4% quinine sulfate carries out assay.
Standard solution preparation: precision takes by weighing the 25.0mg standard items, places the 10ml volumetric flask, adds that mobile phase is ultrasonic to be made sample dissolution and be settled to scale mark.
Testing sample preparation: precision takes by weighing the quinine sulfate sample that 25.0mg India buys, and places the 10ml volumetric flask, adds that mobile phase is ultrasonic to be made sample dissolution and be settled to scale mark.
Standard solution and testing sample are prepared 3 respectively, measure respectively 5 μ l and advance chromatographic column, and the gained peak area is averaged and brought above-mentioned formula calculating, result of calculation such as table 2 into.
Wherein, chromatographic column: C18 (4.6 * 250mm5 μ m); Mobile phase is methyl alcohol-1% potassium dihydrogen phosphate=40: 60, and it is 4 that phosphoric acid is transferred mobile phase PH; Chromatogram temperature: 25 ℃; Sample size: 5 μ l; Flow velocity: 1.0ml/min; Detecting device is UV-detector; Detect wavelength: 316nm.
Table 2 India sample determination result such as following table
It is good, with a high credibility to show that by above-mentioned two examples the present invention detects the quinine sulfate stable content, is applicable to the content detection of quinine sulfate.Quinine sulfate standard items liquid chromatogram is seen accompanying drawing 2.
Methodological study of the present invention
(1) linear relationship is investigated
According to method preparation quinine sulfate standard solution described above, injection liquid chromatography behind 0.2 μ m filtering with microporous membrane, measure according to the method for the invention, difference sample introduction 1 μ l, 2 μ l, 3 μ l, 4 μ l, 5 μ l under condition as described below, data regression gets r=1 to sample size and peak area regression equation.As seen the linear relationship of this method is fine, sees accompanying drawing 3.
Wherein, chromatographic column: C18 (4.6 * 250mm5 μ m); Mobile phase is methyl alcohol-1% potassium dihydrogen phosphate=40: 60, and it is 4 that phosphoric acid is transferred mobile phase PH; Chromatogram temperature: 25 ℃; Sample size: 5 μ l; Flow velocity: 1.0ml/min; Detecting device is UV-detector; Detect wavelength: 316nm.
(2) range of linearity is investigated
Precision takes by weighing quinine sulfate standard items 25.0mg, makes the storing solution that concentration is 2.5mg/ml with mobile phase ultrasonic dissolution constant volume.Add the standard solution that mobile phase is diluted to respectively 0.5 μ g/ml, 1 μ g/ml, 5 μ g/ml, 10 μ g/ml, 20 μ g/ml, 50 μ g/ml, 100 μ g/ml, according to analytical approach of the present invention, sample concentration (X) and peak area (Y) are carried out data regression, getting regression equation is: Y=1.2781X+0.0407, see accompanying drawing 4 for details.The result shows that quinine sulfate is in 0.5 μ g/ml～100 μ g/ml concentration ranges, and peak area and its concentration are good linear relationship.
Wherein, chromatographic column: C18 (4.6 * 250mm5 μ m); Mobile phase is methyl alcohol-1% potassium dihydrogen phosphate=40: 60, and it is 4 that phosphoric acid is transferred mobile phase PH; Chromatogram temperature: 25 ℃; Sample size: 5 μ l; Flow velocity: 1.0ml/min; Detecting device is UV-detector; Detect wavelength: 316nm.
(3) precision is investigated
Press the method for the quinine sulfate standard solution of above-mentioned preparation, the quinine sulfate standard items are repeated sample introduction 6 times, by analytical approach of the present invention, chromatographic condition sample introduction as described below, the result is through 6 revision tests, and the gained peak area value sees the following form, peak area RSD=0.59%.The result shows: it is high that the present invention detects quinine sulfate content precision, favorable reproducibility, and relative standard deviation is little.
The result of table 3 quinine sulfate repeated experiments
Wherein, chromatographic column: C18 (4.6 * 250mm5 μ m); Mobile phase is methyl alcohol-1% potassium dihydrogen phosphate=40: 60, and it is 4 that phosphoric acid is transferred mobile phase PH; Chromatogram temperature: 25 ℃; Sample size: 5 μ l; Flow velocity: 1.0ml/min; Detecting device is UV-detector; Detect wavelength: 316nm.
Claims (6)
1. the present invention is intended to adopt high performance liquid chromatography (HPLC) to measure the content of quinine sulfate, selecting high performance liquid chromatograph is U.S. Agilent-1260, described liquid-phase chromatographic column is C18, mobile phase is that the volume ratio that methyl alcohol and the mixing of 1% potassium dihydrogen phosphate form is 38-42: 62-58, and it is 4 that phosphoric acid is transferred mobile phase PH; UV-detector.
2. the method for claim 1 is characterized in that, high performance liquid chromatography adopts external standard method to carry out the assay of quinine sulfate.
3. the method for claim 1 is characterized in that, described chromatographic column is: C18 (4.6 * 250mm5 μ m), and take octadecylsilane chemically bonded silica as filling agent.
4. the method for claim 1 is characterized in that, described mobile phase mixes the volume ratio that forms as 38-42 take methyl alcohol with 1% potassium dihydrogen phosphate: 62-58, it is 4 that phosphoric acid is transferred mobile phase PH, volume ratio further preferred 40: 60.
5. the method for claim 1 is characterized in that, the detection wavelength is 316nm, and column temperature is 25 ℃, and flow velocity is 1.0ml/min, and sampling volume is 5 μ l.
6. the method for claim 1 is characterized in that, the sample solution of mobile phase excusing from death dissolving preparation, and sample concentration is 2.5mg/ml.
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Citations (1)
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| 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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| 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 |
|---|
| A.S.SIDHU 等: "GENERAL METHOD FOR THE ANALYSIS OF PHARMACEUTICAL DOSAGE FORMS BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY", 《JOURNAL OF CHROMATOGRAPHY》, vol. 391, 31 December 1987 (1987-12-31), pages 233 - 242, XP026550016, DOI: doi:10.1016/S0021-9673(01)94319-5 * |
| MARIA CRISTINA GAUDIANO 等: "Development and validation of a reversed-phase LC method for analysing potentially counterfeit antimalarial medicines", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》, vol. 42, no. 1, 11 September 2006 (2006-09-11), pages 132 - 135 * |
| 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 * |
| 付国家 等: "药用活性炭对硫酸奎宁吸附性能的研究", 《青岛科技大学学报（自然科学版）》, vol. 32, no. 6, 31 December 2011 (2011-12-31), pages 610 - 613 * |
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Application publication date: 20131016 |