CN102590123A - Method for detecting content of bismuth in bismuth potassium citrate medicament - Google Patents

Abstract

The invention relates to a method for detecting the content of bismuth in a bismuth potassium citrate medicament. According to the method, a sample is dissolved with acid; and the content of the bismuth in the bismuth potassium citrate medicament is determined by adopting an air-acetylene flame atomic absorption spectrometry and a bismuth hollow cathode lamp according to the absorption of a bismuth element in the medicament for a bismuth characteristic line. The method for detecting the content of the bismuth in the bismuth potassium citrate medicament by adopting the atomic absorption spectrometry is free from troublesome pretreatment, fewer in reagent types, simple in solution preparation and simple and quick in operation; and in addition, the method has the advantages of favorable selectivity and reproducibility, high accuracy, consistent measuring result with that of an official method, satisfaction in result and practical value.

Description

The detection method of bi content in the CBS medicine

Technical field

The invention belongs to the atomic absorption spectroscopy technical field, relate to a kind of Determination of Bismuth by Atomic Absorption content detecting method of utilizing.

Background technology

Bismuth potassium citrate is a kind of antiulcer drug, is used to treat gastric ulcer, duodenal ulcer, complex ulcer, multiple ulcer and marginal ulcer etc.The Main Ingredients and Appearance of bismuth potassium citrate is a CBS, is a kind of indefinite bismuth-containing compound of forming, and auxiliary material is sweet mellow wine, sodium carboxymethyl cellulose.Bismuth can form one deck bismuth-protein coagulating film at the ulcer surface of stomach, protects its erosion of avoiding hydrochloric acid in gastric juice and proteinase, promotes the ulcer surface healing.But just because of this, also caused long-term, the chronic absorption of bismuth, bismuth is put aside in vivo.If bismuth deposit is in brain, symptoms such as headache, insomnia, failure of memory can appear in the lighter, and weight person then can cause convulsions, dementia etc.Hence one can see that, and bi content is an important indicator of stomach medicine quality control in the stomach medicine.

At present Determination of Bi content method in the stomach medicine is generally adopted compleximetry.Compleximetry is except the required EDTA standard solution of needs preparation experiment; Also need prepare damping fluid, indicator, shelter liquid and in order to the standard reagent solution of demarcating the EDTA standard solution etc.; Need the solution kind of preparation more, operating process is loaded down with trivial details, and sample and solvent-oil ratio are big; Main is that manual titration's terminal point is not easy to control, and operating process is prone to cause component loss to be measured.

Summary of the invention

The detection method that the purpose of this invention is to provide bi content in a kind of CBS medicine, this method adopt the bi content in the aas determination CBS medicine, and method is easy, quick, measure accurately.

The detection method of bi content is after sample is dissolved with acid in the CBS medicine provided by the invention; Adopt the Air-acetylene Flame atomic absorption spectrography (AAS); Through adopting Bi hollow cathode lamp, thereby the new method that flame atomic absorption spectrometry is measured bi content in the CBS medicine has been set up in the absorption of the characteristic spectral line of bismuth according to bismuth element in the medicine.

The detection method step of bi content is following in the CBS medicine of the present invention:

1) accurately takes by weighing quantitative high purity bismuth,, move in the volumetric flask, with the deionized water constant volume, as the bismuth standard reserving solution with the dissolving of 1: 1 salpeter solution of volume ratio; Accurately pipetting the bismuth standard reserving solution of certain volume, further is 5% HNO with percent by volume ₃The solution dilution constant volume is mixed with the bismuth standard solution of a series of variable concentrations;

2) accurately take by weighing quantitative CBS drug sample,, add 1: 1 salpeter solution of volume ratio again, with deionized water constant volume in volumetric flask, as the sample storing solution with the low amounts of water dissolving; Accurately pipetting the sample storing solution of certain volume, further is 5% HNO with percent by volume ₃The solution dilution constant volume is mixed with sample solution; Do not add simultaneously sample, according to same reagent and consumption preparation sample blank liquid;

3) use flame atomic absorption spectrophotometer and Bi hollow cathode lamp, regulate spectrophotometer wavelength 223.1nm, lamp current 3mA, spectral band-width 0.4nm, acetylene flow 1.2L/min, air mass flow 6.5L/min;

4) proofread and correct spectrophotometer zero point with sample blank liquid, measure the absorbance of variable concentrations bismuth standard solution, obtain the typical curve of bismuth standard solution; The light absorption value of working sample solution calculates the bi content in the CBS drug sample according to typical curve simultaneously.

The present invention has investigated solution acidity and coexisting substances to measuring result's influence.

1) influence of solution acidity (influence of the concentration of acid)

Select same testing sample, change the concentration that sample dissolution is used salpeter solution, under identical instrument condition, test, the result finds that absorbance increases with the increase of sample solution acidity.Consider that salpeter solution itself maybe be to the influence of absorbance, experiment again obtains result shown in Figure 1 after the salpeter solution that uses respective concentration rectifies an instrument zero point.Experiment shows, can improve its absorbance with salpeter solution dissolving bismuth ion, but the concentration of acid is little to the absorbance influence of bismuth ion within the specific limits.Consider the steady dissolution problem of sample and the protection problem of instrument itself, the present invention selects 5% salpeter solution.

2) influence of coexisting substances

The present invention is a benchmark with 4 μ g/mL bismuth standard solution under selected condition, adds the interfering material of different amounts, measure by inventive method, and be standard with error less than 5%.The result shows: 2 times Al ³⁺, 50 times Cl ^-, K ⁺, Ca ²⁺, PO ₄ ^3-, Mg ²⁺, Na ⁺, 100 times Cu ²⁺, SiO ₃ ^2-, NaHSO ₃, EDTA, sweet mellow wine, glucose, halfcystine etc. are all noiseless.This shows that interpolation material common in the medicine does not disturb Determination of Bi content in the inventive method.

The present invention also investigates each item performance index of foundation test method.

1) range of linearity of typical curve and linear relationship

Under the optimization experiment condition; The inventive method is in bismuth concentration of standard solution 2～20 μ g/mL scopes; The concentration of bismuth solution and its absorbance are good linear relationship, and equation of linear regression is A=0.0172C+0.0021 (the μ g/mL of unit of concentration C), linearly dependent coefficient r=0.9996 (R ²=0.9993, behind evolution, get r=0.9996).

2) replica test

To bi concns is the continuous replicate determination of standard reference material solution 9 times of 4.00 μ g/mL, and its relative standard deviation RSD is 0.34%.

3) sensitivity (detection limit) test

Under optimal conditions, measure blank value (n=11) and standard series, draw the standard deviation of blank value and the slope of typical curve, according to the IUPAC regulation, calculate detecting of bismuth element and be limited to 0.084 μ g/mL (S/N=3).

4) recovery test

Carry out the recovery of standard addition experiment in the process that the same sample solution of variable concentrations is measured, the recovery between 104.3%～108.0%, average recovery of standard addition 106.2%, the RSD of the recovery is 1.7%.

5) control test

Measurement result of the present invention and version NF method (compleximetry) result that surveys in 2010 compare, and the result is consistent.

The detection method of bi content and traditional compleximetry compare in the CBS medicine that the present invention sets up, and its advantage is mainly reflected in following several respects:

1) required reagent type is few, and the solution preparation is simple.The inventive method only needs two kinds of reagent of high purity bismuth and high pure nitric acid except that measuring medicine, the preparation of standard solution and sample solution only need quantitatively take by weighing a certain amount of, gets final product with certain density salpeter solution dilution, constant volume;

2) simple and efficient to handle.The inventive method only needs can measure after input instrument condition and standard solution, the sample solution information after preparing standard solution and sample solution.Because solution is automatic suction, and apparatus preparation has the Computer Analysis computing function, and analysis speed is very fast, can draw analysis result in tens minutes;

3) selectivity is high.Because the inventive method is under optimal conditions, directly to measure the characteristic spectral line of bismuth element in the medicine, so disturb less, selectivity is high, the influence experiment of relevant coexisting substances has proved fully that also common interpolation material in the medicine does not disturb the mensuration of bismuth;

4) reappearance is high, good stability.Combustion gas in the device burner and combustion-supporting gas are premixs, so flameholding, data reappearance is good, precision is high.The RSD of replica test substantive approach is 0.34%;

5) accuracy is high.The recovery of standard addition assay shows average recovery of standard addition 106.2%, and RSD is 1.4%; On the other hand, measurement result of the present invention with 2010 version NF method (compleximetry) to survey the result consistent.

The detection method of bi content need not loaded down with trivial details pre-treatment in the CBS medicine that the present invention sets up, and only need take by weighing an amount of sample, after acid is dissolved, can carry out assay determination; Method is easy, sensitive, quick; Not only save reagent, and selectivity is good, favorable reproducibility, accuracy high, measurement result is consistent with official method; The result is satisfactory, and is with practical value.

Description of drawings

Fig. 1 is the influence of salpeter solution concentration (%) to absorbance.

Fig. 2 is the standard working curve of embodiment 1.

Embodiment

Embodiment 1

The bismuth potassium citrate granule of producing with Livzon Pharmaceutical Factory, Livzon Group (batch number 0910190) is an example.

1, the preparation of bismuth standard reserving solution: precision takes by weighing the 0.2500g bismuth metal and places beaker, adds 1: 1 HNO of volume ratio ₃Solution 25mL dissolving in the 250mL volumetric flask, obtains the bismuth standard reserving solution of acidity 5%, concentration 1000 μ g/mL with the deionized water constant volume.

2, the preparation of bismuth standard analysis liquid: pipette 10.00mL bismuth standard reserving solution in the 100mL volumetric flask, with 5%HNO ₃The solution constant volume is mixed with the bismuth standard analysis liquid of concentration 100 μ g/mL.

3, the preparation of bismuth standard solution: in 7 50mL volumetric flasks, pipette 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 10.00mL bismuth standard analysis liquid respectively, with 5%HNO ₃The solution constant volume is mixed with the bismuth standard solution series that concentration is respectively 0 μ g/mL, 2 μ g/mL, 4 μ g/mL, 6 μ g/mL, 8 μ g/mL, 10 μ g/mL, 20 μ g/mL.

4, the preparation of sample storing solution: precision takes by weighing bismuth potassium citrate (bismuth citrate k particle) 2.2305g in the small beaker of cleaning, after separating so that 50mL is water-soluble, adds 1: 1 HNO of volume ratio again ₃Solution 25mL, with the deionized water constant volume in the 250mL volumetric flask.

5, the preparation of sample solution: pipette bismuth potassium citrate sample storing solution 10.00mL, with 5%HNO ₃The solution constant volume is in the 100mL volumetric flask.

6, the preparation of sample blank liquid:, prepare sample blank liquid according to step 4,5 same reagent and consumptions except that not adding the sample.

7, the preparation of sample analysis liquid and sample mark-on liquid: in 6 50mL volumetric flasks, pipette each two parts of 2.00mL, 3.00mL, 4.00mL sample solution respectively, a copy of it is with 5% HNO ₃The solution constant volume is mixed with No. 1 sample analysis liquid, No. 2 sample analysis liquid and No. 3 sample analysis liquid, is used for the mensuration of sample; All add 2.00mL bismuth standard analysis liquid again in another part, with 5% HNO ₃The solution constant volume is mixed with No. 1 sample mark-on liquid, No. 2 sample mark-on liquid and No. 3 sample mark-on liquid, is used for the mensuration of the recovery.

8, instrument condition setting: use WFX-120 or flame atomic absorption spectrophotometer, Bi hollow cathode lamp of the same type; Measure with ethyne-air flame, regulate spectrophotometer wavelength 223.1nm, lamp current 3mA, spectral band-width 0.4nm, burner height 7mm, acetylene pressure 0.09MPa, acetylene flow 1.2L/min, air pressure 0.3MPa, air mass flow 6.5L/min.

9, sample determination: after instrument condition and input standard solution series and sample analysis liquid information are set; The instrument igniting; Proofread and correct spectrophotometric zero point with sample blank liquid; The absorbance of sequentially determining standard solution series and sample analysis liquid, sample mark-on liquid, instrument can be quoted the bi content in working curve equation (Fig. 2) and the sample solution automatically according to the information of absorbance and input.

Sample concentration (μ g/mL) is changed the massfraction (g/g) with bismuth-containing in the solid medicine, and testing result is seen table 1.Bi content mean value in the bismuth potassium citrate sample is 0.1178 g/g (n=3), average recovery of standard addition 106.2% (n=3).

Embodiment 2

Be further check embodiment 1 precision of analysis, adopt that version NF method in 2010---compleximetry is measured embodiment 1 sample, two kinds of methods and results differences of comparison.

Compound concentration is about the EDTA solution of 0.05mol/L, with 0.05000mol/L Zn ²⁺Standard solution is demarcated, and obtaining accurate concentration is the EDTA standard solution of 0.04996mol/L.

Accurately take by weighing a certain amount of bismuth potassium citrate medicine, separate, add 1: 1 HNO of volume ratio again so that 50mL is water-soluble ₃Solution 25mL dissolving, the deionized water constant volume is in the 250mL volumetric flask.

Draw above-mentioned sample solution 25.00mL, carry out complexometry with the EDTA standard solution by official method, experimental result is listed in the table 2.

Claims (1)

1. the detection method of bi content in the CBS medicine is characterized in that detecting according to following method:

1) accurately takes by weighing quantitative high purity bismuth,, move in the volumetric flask, with the deionized water constant volume, as the bismuth standard reserving solution with the dissolving of 1: 1 salpeter solution of volume ratio; Accurately pipetting the bismuth standard reserving solution of certain volume, further is 5% HNO with percent by volume ₃The solution dilution constant volume is mixed with the bismuth standard solution of a series of variable concentrations;

2) accurately take by weighing quantitative CBS drug sample,, add 1: 1 salpeter solution of volume ratio again, with deionized water constant volume in volumetric flask, as the sample storing solution with the low amounts of water dissolving; Accurately pipetting the sample storing solution of certain volume, further is 5% HNO with percent by volume ₃The solution dilution constant volume is mixed with sample solution; Do not add simultaneously sample, according to same reagent and consumption preparation sample blank liquid;

3) use flame atomic absorption spectrophotometer and Bi hollow cathode lamp, regulate spectrophotometer wavelength 223.1nm, lamp current 3mA, spectral band-width 0.4nm, acetylene flow 1.2L/min, air mass flow 6.5L/min;

4) proofread and correct spectrophotometer zero point with sample blank liquid, measure the absorbance of variable concentrations bismuth standard solution, obtain the typical curve of bismuth standard solution; The light absorption value of working sample solution calculates the bi content in the CBS drug sample according to typical curve simultaneously.

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