CN104880444A - Method for determining kanamycin sulfate - Google Patents
Method for determining kanamycin sulfate Download PDFInfo
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- CN104880444A CN104880444A CN201510260027.9A CN201510260027A CN104880444A CN 104880444 A CN104880444 A CN 104880444A CN 201510260027 A CN201510260027 A CN 201510260027A CN 104880444 A CN104880444 A CN 104880444A
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Abstract
The invention discloses a method for determining kanamycin sulfate. The method comprises the following steps: adding 0.0, 0.1, 0.5, 0.8, 1.0, 1.2mL of 10.microng/mL kanamycin sulfate solution in 6 10mL colorimetric tubes, adding 0.3-1.5mL of a Britton-Robinson buffer solution with the pH of 6.0 and 0.5-2.0mL of a 2.0*10<-5>mol/L tetra carboxylic-zinc phthalocyanine solution, diluting to the scale by secondary distilled water, and shaking evenly; reacting for 10 minutes at room temperature, and scanning a resonance scattering spectroscopy by a 1cmquartz colorimetric utensil by a mode of lambda ex=lambda em; determining the resonance scattering intensity I332nm of the solution with kanamycin sulfate and the resonance scattering intensity I0 of the reagent blank at the 332nm part, and calculating the difference value delta I332nm=I332nm-I0; and diluting kanamycin sulfate eye drops or kanamycin sulfate injection, determining the resonance scattering intensity by the same method, and calculating the content of kanamycin sulfate in th eye drops or the injection. The method is high in flexibility, is good in selectivity, and is simple, convenient and rapid.
Description
Technical field
The present invention relates to the assay method of kanamycin sulfate, particularly utilize tetracarboxylic ZnPc to measure the resonance scattering spectrometry of kanamycin sulfate.
Background technology
Kanamycin sulfate (Kanamycin Sulfate, KANA) be a kind of aminoglycoside broad-spectrum antibiotic, the severe infections mainly caused as Escherichia coli, Proteus, pneumobacillus etc. gram-negative bacteria is effective in cure, also can be used as Second line Drug to treat tuberculosis, is anti-infectives important clinically.But antibiotic abuse can cause serious adverse consequences, clinically strict control is needed for antibiotic using dosage, therefore, the quantitative measurement of kanamycins is had very important significance.The assay method being usually used in kanamycins has microbial method, high performance liquid chromatography, spectrophotometric method, polarimetry, colourimetry, electrochemical process, resonance scattering spectrometry etc.Wherein resonance scattering spectrometry have easy and simple to handle, highly sensitive, selectivity is good, analyze the advantages such as quick, in Pharmaceutical Analysis, had some to apply in recent years.Tetracarboxylic ZnPc (ZnC
4pc) similar is in porphyrin, ionic associate can be formed with kanamycin sulfate by electrostatic attraction effect in weakly acidic solution, the resonance scattering intensity of system is increased, and there is not been reported for the method for the Resonance Scattering Spectrometric Determination kanamycin sulfate set up accordingly.
Summary of the invention
The object of this invention is to provide a kind of resonance scattering spectrometry utilizing tetracarboxylic ZnPc to measure kanamycin sulfate.
Concrete steps are:
In 6 10mL color comparison tubes, add 0.0 respectively, 0.1,0.5,0.8,1.0,1.2mL 10.0 μ g/mL kanamycin sulfate solution, again often prop up in color comparison tube the Bloomsbury adding 0.3 ~ 1.5mL pH6.0 smooth-Robison (Britton-Robinson, B-R) buffer solution and 0.5 ~ 2.0mL 2.0 × 10
-5mol/L tetracarboxylic ZnPc solution, is diluted to scale with redistilled water, shakes up, and reacts after 10 minutes, scan resonance scattering spectroscopy with 1cm quartz colorimetric utensil on fluorophotometer in the mode of λ ex=λ em under room temperature; The resonance scattering intensity I of the solution being added with kanamycin sulfate is measured respectively at 332nm place
332nmdo not add the resonance scattering intensity I of the blank reagent solution of kanamycin sulfate
0, calculated difference Δ I
332nm=I
332nm-I
0, difference DELTA I
332nmlinear within the scope of 0.1 ~ 1.2 μ g/mL with kanamycin sulfate concentration C, equation of linear regression is Δ I
332nm=19.43 C-2.201, related coefficient 0.9922, detection limit 0.029 μ g/mL; Separately get Kanamycin sulfate eye drops or kanamycin sulfate injection liquid, dilute with water obtains the solution that concentration is 400 μ g/mL; Again this solution dilution is obtained the liquid to be measured of 10 μ g/mL; Get 1 ~ 3 mL liquid to be measured, be measured in the same method resonance scattering intensity, calculate the content of kanamycin sulfate in Kanamycin sulfate eye drops or parenteral solution.
Assay method of the present invention is highly sensitive, selectivity good, easy, quick.
Accompanying drawing explanation
Fig. 1 is the resonance light scattering spectrogram of embodiment of the present invention blank and 1 μ g/mL kanamycin sulfate.
Mark in figure: a: blank; B: blank+1 μ g/mL KANA.
Embodiment
Embodiment:
In 6 10mL color comparison tubes, add 0.0 respectively, 0.1,0.5,0.8,1.0,1.2mL 10.0 μ g/mL kanamycin sulfate solution, then often prop up in color comparison tube the Bloomsbury adding 1.0mL pH6.0 smooth-Robison's buffer solution and 1.3mL 2.0 × 10
-5mol/L tetracarboxylic ZnPc solution, is diluted to scale with redistilled water, shakes up, and reacts after 10 minutes, scan resonance scattering spectroscopy with 1cm quartz colorimetric utensil on fluorophotometer in the mode of λ ex=λ em under room temperature; The resonance scattering intensity I of the solution being added with kanamycin sulfate is measured respectively at 332nm place
332nmdo not add the resonance scattering intensity I of the blank reagent solution of kanamycin sulfate
0, calculated difference Δ I
332nm=I
332nm-I
0, difference DELTA I
332nmlinear within the scope of 0.1 ~ 1.2 μ g/mL with kanamycin sulfate concentration C, equation of linear regression is Δ I
332nm=19.43C-2.201, related coefficient 0.9922, detection limit 0.029 μ g/mL; Separately get Kanamycin sulfate eye drops 8mL and put into 100mL volumetric flask or kanamycin sulfate injection liquid 1mL puts into 250mL volumetric flask, be diluted with water to scale, shake up.Then respectively get the above-mentioned solution of 2.5mL and put into 100mL volumetric flask respectively, be diluted with water to scale, shake up, as liquid to be measured.Get the above-mentioned liquid to be measured of 1mL respectively and be measured in the same method resonance scattering intensity level, and carry out recovery experiment, the results are shown in Table 1.
kanamycin sulfate sample determination result (n=5)
| Sample | Measured value (g/L) | Labelled amount (g/L) | The recovery (%) | RSD(%) |
| Eye drops | 4.98 | 5 | 108.3 | 1.1 |
| Parenteral solution | 243.0 | 250 | 104.3 | 0.25 |
Claims (1)
1. measure a method for kanamycin sulfate, it is characterized in that concrete steps are:
In 6 10mL color comparison tubes, add 0.0 respectively, 0.1,0.5,0.8,1.0,1.2mL 10.0 μ g/mL kanamycin sulfate solution, then often prop up in color comparison tube the Bloomsbury adding 0.3 ~ 1.5mL pH6.0 smooth-Robison and Britton-Robinson buffer solution and 0.5 ~ 2.0mL 2.0 × 10
-5mol/L tetracarboxylic ZnPc solution, is diluted to scale with redistilled water, shakes up, and reacts after 10 minutes, scan resonance scattering spectroscopy with 1cm quartz colorimetric utensil on fluorophotometer in the mode of λ ex=λ em under room temperature; The resonance scattering intensity I of the solution being added with kanamycin sulfate is measured respectively at 332nm place
332nmdo not add the resonance scattering intensity I of the blank reagent solution of kanamycin sulfate
0, calculated difference Δ I
332nm=I
332nm-I
0, difference DELTA I
332nmlinear within the scope of 0.1 ~ 1.2 μ g/mL with kanamycin sulfate concentration C, equation of linear regression is Δ I
332nm=19.43 C-2.201, related coefficient 0.9922, detection limit 0.029 μ g/mL; Separately get Kanamycin sulfate eye drops or kanamycin sulfate injection liquid, dilute with water obtains the solution that concentration is 400 μ g/mL; Again this solution dilution is obtained the liquid to be measured of 10 μ g/mL; Get 1 ~ 3 mL liquid to be measured, be measured in the same method resonance scattering intensity, calculate the content of kanamycin sulfate in Kanamycin sulfate eye drops or parenteral solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108254344A (en) * | 2018-01-03 | 2018-07-06 | 桂林理工大学 | A kind of method that melamine is measured using crystal violet |
| CN108318456A (en) * | 2018-01-03 | 2018-07-24 | 桂林理工大学 | A method of roxithromycin is measured based on eosin |
| CN114113018A (en) * | 2021-11-30 | 2022-03-01 | 厦门大学 | Fluorescence detection method for determining zinc ions by taking tetranitrophthalocyanine as reagent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103175818A (en) * | 2013-03-19 | 2013-06-26 | 桂林理工大学 | Method for detecting melamine |
| CN103439307A (en) * | 2013-09-30 | 2013-12-11 | 桂林理工大学 | Method for rapidly detecting protein in food by using indigo dye |
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2015
- 2015-05-21 CN CN201510260027.9A patent/CN104880444A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103175818A (en) * | 2013-03-19 | 2013-06-26 | 桂林理工大学 | Method for detecting melamine |
| CN103439307A (en) * | 2013-09-30 | 2013-12-11 | 桂林理工大学 | Method for rapidly detecting protein in food by using indigo dye |
Non-Patent Citations (2)
| Title |
|---|
| JIANG Z L等: "Determination of Trace Gentamycin by Resonance Scattering Spectral Method", 《SICHUAN NORMAL UNIV》 * |
| 王高等: "基于共振瑞利散射血清蛋白浓度检测的研究", 《光谱学与光谱分析》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108254344A (en) * | 2018-01-03 | 2018-07-06 | 桂林理工大学 | A kind of method that melamine is measured using crystal violet |
| CN108318456A (en) * | 2018-01-03 | 2018-07-24 | 桂林理工大学 | A method of roxithromycin is measured based on eosin |
| CN114113018A (en) * | 2021-11-30 | 2022-03-01 | 厦门大学 | Fluorescence detection method for determining zinc ions by taking tetranitrophthalocyanine as reagent |
| CN114113018B (en) * | 2021-11-30 | 2023-10-24 | 厦门大学 | Fluorescent detection method for measuring zinc ions by taking tetranitrophthalocyanine as reagent |
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Application publication date: 20150902 |