CN108254345A - A kind of method that roxithromycin is measured based on phloxine - Google Patents

A kind of method that roxithromycin is measured based on phloxine Download PDF

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Publication number
CN108254345A
CN108254345A CN201810004921.3A CN201810004921A CN108254345A CN 108254345 A CN108254345 A CN 108254345A CN 201810004921 A CN201810004921 A CN 201810004921A CN 108254345 A CN108254345 A CN 108254345A
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CN
China
Prior art keywords
roxithromycin
scattering strength
concentration
added
ethyl alcohol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810004921.3A
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Chinese (zh)
Inventor
唐宁莉
范晶晶
马小龙
王文平
师蓉
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Guilin University of Technology
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Guilin University of Technology
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Filing date
Publication date
Application filed by Guilin University of Technology filed Critical Guilin University of Technology
Priority to CN201810004921.3A priority Critical patent/CN108254345A/en
Publication of CN108254345A publication Critical patent/CN108254345A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6428Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N2021/6417Spectrofluorimetric devices

Abstract

The invention discloses a kind of methods that roxithromycin is measured based on phloxine.In 8 colorimetric cylinders, be separately added into 0.0,0.05,0.1,0.5,1.0,1.5,2.0,2.5mL 0.05mg/L roxithromycin, it is separately added into phloxine and acetic acid, it is settled to 10 mL, after reaction, with 1cm cuvettes on fluophotometer in a manner of λ ex=λ em scanning optical spectrum, measure the scattering strength I and I added with roxithromycin and the blank for being not added with roxithromycin respectively at 327 nm0, calculate scattering strength difference △ I=I I0.Roxithromycin capsules is taken to be dissolved with absolute ethyl alcohol, is filtered, is settled to 100mL, 5mL is taken to be settled to 50mL with ethyl alcohol, 0.5mL ethyl alcohol is taken to be settled to 50mL as prepare liquid, scattering strength value is measured in the same method, calculates the content of roxithromycin in capsule.The method of the present invention is easy, high sensitivity.

Description

A kind of method that roxithromycin is measured based on phloxine
Technical field
The present invention relates to the assay methods of roxithromycin, are based particularly on the resonance scattering that phloxine measures roxithromycin Spectroscopic methodology.
Background technology
Roxithromycin (ROX) is at present clinically using the excellent novel erythromycin product of extensive, curative effect, it is to golden yellow Portugal Grape coccus, staphylococcus epidermis, streptococcus pneumonia, enterococcus, anaerobic bacteria, mycoplasma pneumoniae, Chlamydia, gonococcus etc. have anti- Bacterium acts on, and can reach and thoroughly treats effect uneasy to recur.The method for measuring roxithromycin content at present mainly has biological standardization Method, spectrophotometry and chromatography etc..Resonance scattering spectrometry has the characteristics that easy quick, high sensitivity, detection limit are low, closely Trace analysis is had been used for over year, but by the use of phloxine as probe, the method that roxithromycin is measured using resonance scattering technology There is not been reported.This patent reacts to form ionic associate in an acidic solution using roxithromycin and phloxine, leads Cause system resonance scattering intensity significantly increases, and it is good to establish a kind of selectivity accordingly, and easy, accurate, sensitive to measure Luo Hong mould The resonance scattering spectroscopy new method of element.
Invention content
The object of the present invention is to provide the resonance scattering spectrometries that a kind of phloxine measures roxithromycin.
The specific steps are:
In the colorimetric cylinder of 8 10mL, be separately added into 0.0,0.05,0.1,0.5,1.0,1.5,2.0,2.5mL it is a concentration of The roxithromycin of 0.05mg/L, then be separately added into 8 colorimetric cylinders a concentration of 0.001mol/L of 1.0mL phloxine and The acetic acid of a concentration of 0.02mol/L of 2.0mL is settled to 10mL with ultra-pure water, is reacted at 45 DEG C after ten minutes, with 1cm cuvettes In on fluophotometer in a manner of λ ex=λ em scanning optical spectrum, measured respectively at 327nm added with roxithromycin solution dissipate It penetrates intensity I and is not added with the scattering strength I of the blank solution of roxithromycin0, calculate the difference △ I=I-I of scattering strength0, scattering Strength difference △ I are with roxithromycin concentration c 2.5 × 10-4~1.25 × 10-2In good linear relationship, line in the range of mg/L Property regression equation is:△ I=2.586 × 104C+35.13, correlation coefficient r=0.9971, detection are limited to 1.82 × 10-4mg/L。
Roxithromycin capsules 1 separately are taken, weigh 0.0050g, are dissolved with 20mL absolute ethyl alcohols, filtering, filtrate ultra-pure water Then constant volume takes the ethyl alcohol constant volume that the above-mentioned solution mass percent concentrations of 5mL are 20% to hold in 50mL in 100mL volumetric flasks In measuring bottle, then the ethyl alcohol constant volume that the solution 0.5mL mass percent concentrations after dilution is taken to be 20% is made in 50mL volumetric flasks For prepare liquid, 0.7mL prepare liquids is taken to be measured in the same method scattering strength value, calculate the content of roxithromycin in roxithromycin capsules.
Assay method of the present invention is fast and simple, high sensitivity.
Description of the drawings
Fig. 1 is blank of the embodiment of the present invention and 5.0 × 10-3The resonance light scattering spectrogram of mg/L roxithromycin.
It is marked in figure:a:Blank;b:Blank -5.0 × 10-3mg/L ROX。
Specific embodiment
Embodiment:
In the colorimetric cylinder of 8 10mL, be separately added into 0.0,0.05,0.1,0.5,1.0,1.5,2.0,2.5mL it is a concentration of The roxithromycin of 0.05mg/L, then be separately added into 8 colorimetric cylinders a concentration of 0.001mol/L of 1.0mL phloxine and The acetic acid of a concentration of 0.02mol/L of 2.0mL, 10mL is settled to ultra-pure water, it is reacted at 45 DEG C after ten minutes, with 1cm cuvettes In on fluophotometer in a manner of λ ex=λ em scanning optical spectrum, measured respectively at 327nm added with roxithromycin solution dissipate It penetrates intensity I and is not added with the scattering strength I of the blank solution of roxithromycin0, calculate the difference △ I=I-I of scattering strength0, scattering Strength difference △ I are with roxithromycin concentration c 2.5 × 10-4~1.25 × 10-2In good linear relationship, line in the range of mg/L Property regression equation is:△ I=2.586 × 104C+35.13, correlation coefficient r=0.9971, detection are limited to 1.82 × 10-4mg/L。 Take what the peaceful phoenix Pharmacy stock Co., Ltd (sample 1) in Zhuhai and Jiangsu Fubang .Pharm Co., Ltd.'s (sample 2) produced respectively Each (specification of roxithromycin capsules:150mg/), 0.0050g samples are weighed respectively in beaker, with 20mL absolute ethyl alcohols Dissolving, filtering, filtrate in 100mL volumetric flasks, then take the above-mentioned solution mass percents of 5mL dense respectively with ultra-pure water constant volume Spend the ethyl alcohol constant volume for 20% in 50mL volumetric flasks, then respectively take dilution after solution 0.5mL be with mass percent concentration 20% ethyl alcohol constant volume, as prepare liquid, takes 0.7mL prepare liquids to be measured in the same method scattering strength value respectively in 50mL volumetric flasks, point The content of roxithromycin in roxithromycin capsules is not calculated, the results are shown in Table 1.
Table 1:The measurement result (n=5) of roxithromycin content in roxithromycin capsules

Claims (1)

  1. A kind of 1. method for measuring roxithromycin, it is characterised in that the specific steps are:
    (1) in the colorimetric cylinder of 8 10 mL, be separately added into 0.0,0.05,0.1,0.5,1.0,1.5,2.0,2.5mL it is a concentration of The roxithromycin of 0.05mg/L, then be separately added into 8 colorimetric cylinders a concentration of 0.001mol/L of 1.0 mL phloxine and The acetic acid of a concentration of 0.02mol/L of 2.0mL is settled to 10 mL, after being reacted 10 minutes at 45 DEG C, with 1cm ratios with ultra-pure water Color ware on fluophotometer in a manner of λ ex=λ em scanning optical spectrum, measured respectively added with roxithromycin solution at 327 nm Scattering strength I and be not added with roxithromycin blank solution scattering strength I0, calculate difference △ I=I-I of scattering strength0, Its scattering strength difference △ I are with roxithromycin concentration c 2.5 × 10-4~1.25 × 10-2In good linear in the range of mg/L Relationship, equation of linear regression are:△I=2.586×104C+35.13, correlation coefficient r=0.9971, detection are limited to 1.82 × 10- 4mg/L;
    (2) roxithromycin capsules 1 separately are taken, weighs 0.0050, dissolved with 20mL absolute ethyl alcohols, filtering, filtrate is determined with ultra-pure water It is dissolved in 100mL volumetric flasks, then takes the ethyl alcohol constant volume that the above-mentioned solution mass percent concentrations of 5mL are 20% in 50mL capacity In bottle, then take the solution 0.5mL after dilution by the use of the ethyl alcohol constant volume that mass percent concentration is 20% in 50mL volumetric flasks as treating Liquid is surveyed, takes 0.7mL prepare liquids according to step(1)Method measure scattering strength value, calculate roxithromycin in roxithromycin capsules Content amount.
CN201810004921.3A 2018-01-03 2018-01-03 A kind of method that roxithromycin is measured based on phloxine Pending CN108254345A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102095697A (en) * 2010-12-07 2011-06-15 桂林理工大学 Method for measuring roxithromycin

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102095697A (en) * 2010-12-07 2011-06-15 桂林理工大学 Method for measuring roxithromycin

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
M.I.WALSH ET AL.: "Spectrophotometric Determination of Four Macrolide Antibiotics in Pharmaceutical Formulations and Biological Fluids via Binary Complex Formation with Eosin and Spectrophotometry", 《JOURNAL OF AOAC INTERNATIONAL》 *
周尚 等: "卤代荧光素与西布曲明相互作用的共振散射光谱特征及其分析应用", 《分析测试学报》 *
杨清玲 等: "Ag+-Cl—多取代荧光素体系的RRS和RNLS光谱及其分析", 《中国科学:化学》 *
陈莲惠 等: "对二甲基氨基偶氮苯染料共振瑞利散射法测定红霉素", 《分析试验室》 *

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Application publication date: 20180706