CN102141562B - Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration - Google Patents

Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration Download PDF

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CN102141562B
CN102141562B CN2010102946607A CN201010294660A CN102141562B CN 102141562 B CN102141562 B CN 102141562B CN 2010102946607 A CN2010102946607 A CN 2010102946607A CN 201010294660 A CN201010294660 A CN 201010294660A CN 102141562 B CN102141562 B CN 102141562B
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CN102141562A (en
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郭建宇
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Shanghai Normal University
University of Shanghai for Science and Technology
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Abstract

The invention discloses a method for analyzing the purity of a 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration, and the method belongs to the field of medical intermediate analysis. The quantitative analysis of products is carried out by adopting a method of converting sulfate into hydrochloride which is easily dissolved into water and titrating the total acidity in a solution through strong base. The destination of a titration reaction is indicated through an acid-base indicator or an acidometer, and the recovery rate and precision tests of the method verify that the analysis result of the method is accurate and reliable. The method disclosed by the invention has the advantages of mature method, low cost and simplicity and convenience in operation because an acid base titration analysis method is adopted. The accuracy and precision of the method are high by adopting a macro analysis method.

Description

Titrimetry analyzes 2,4, the method for 5-triamido-6-hydroxy pyrimidine sulfate sample purity
Technical field
The present invention relates to a kind ofly 2,4, the method for 5-triamido-6-hydroxy pyrimidine sulfate sample purity is specially and uses titrimetry to analyze 2,4, and the method for 5-triamido-6-hydroxy pyrimidine sulfate sample purity belongs to the medicine intermediate analysis field.
Background technology
2,4,5-triamido-6-hydroxy pyrimidine sulfate is the important intermediate of synthetic broad-spectrum antiviral drug ACV (acyclovir) and Antianemic Agents folic acid (folic acid), but the analytical approach of its sample does not see that bibliographical information is arranged all the time.At present domestic also have minority enterprise to begin synthetic this intermedium, but owing to lack unified analytical method, so be difficult to this product is carried out quality monitoring.
Summary of the invention
The objective of the invention is in order to provide a kind of titrimetry to analyze 2,4, the method for 5-triamido-6-hydroxy pyrimidine sulfate sample purity is to solve the problems referred to above of prior art.
The object of the invention can be realized through following technical scheme.
A kind of titrimetry analyzes 2,4, and the method for 5-triamido-6-hydroxy pyrimidine sulfate sample purity adopts and converts this sulfate to hydrochloride soluble in water earlier, carries out the product quantitative test with the method for total acidity in the highly basic volumetric soiutions then.
Its concrete steps are following:
1) the HCl WS of preparation 0.1-1.0 mol/L is to be calibrated.
2) the NaOH WS of preparation 0.1-1.0 mol/L is to be calibrated; Take by weighing the NaOH of 5.0 grams, with the dissolved in distilled water of 250mL, to be calibrated.
3) blank test
Use is measured the pH value of distilled water that obtain solution uses through the acidometer of straightened up in place, is designated as pH Blank, and as all titration end-points;
Or only in hydrochloric acid standard solution concentration calibration process, use at obtain solution to drip 1-2 in the distilled water and drip methyl orange indicator, become orange titration end-point of demarcating with HCl WS titration to the indicator color of above-mentioned preparation by yellow as hydrochloric acid;
Or only in NaOH concentration of standard solution calibration process, use at obtain solution to drip 1-2 in the distilled water and drip phenolphthalein indicator, become the titration end-point that pink is demarcated as NaOH with following NaOH WS titration to the indicator color for preparing by colourless.
4) demarcation of HCl concentration of aqueous solution
Precision takes by weighing the anhydrous Na of 0.45-0.55 gram 2CO 3, be designated as W NaCO3, place the beaker of 250mL, add the above-mentioned distilled water of having surveyed the pH value of 100mL, ultrasonic dissolution carries out titration with the aforementioned HCl WS for preparing, with pH BlankAs titration end-point;
Or at this Na 2CO 3Drip 1-2 in the WS and drip methyl orange indicator, become orange by yellow as titration end-point with the color of methyl orange indicator;
Record V Titration(unit: mL), be calculated as follows the concentration C of the HCl WS HCl
Survey three parts of parallel appearance, average
Figure 2010102946607100002DEST_PATH_IMAGE001
。
4) demarcation of the NaOH WS of 0.5mol/L
In the beaker of 250mL, accurately pipette the aforementioned HCl WS of having demarcated concentration of 10mL, add 100mL distilled water, carry out titration with the NaOH WS for preparing, with pH BlankAs titration end-point;
Or in this HCl WS, drip 1-2 and drip phenolphthalein indicator, with the color of phenolphthalein indicator by the colourless pink that becomes as titration end-point;
Record V Titration(unit: mL), be calculated as follows the concentration of the NaOH WS;
Survey three parts of parallel appearance, average
Figure 345362DEST_PATH_IMAGE002
。
5) this sulfate analytical approach is investigated
The precision and the recovery with this this titrimetry of sulfate standard specimen test method.
Accurate 2 of 0.12 gram that takes by weighing in the beaker of 250mL; 4; 5-triamido-6-hydroxy pyrimidine sulfate standard specimen (purity 95%); Be designated as ; Move into the aforementioned HCl WS of having demarcated about 0.5mol/L of concentration of 25mL, and add 40mL distilled water, made it to dissolve in ultrasonic 5 minutes.Carry out titration with the aforementioned NaOH WS of having demarcated about 0.5mol/L of concentration, with pH BlankAs titration end-point;
Or the titration end-point indication changes bromcresol green sodium (the 1g/L WS) into by the acidometer indication: the acid mixture neutralization indicator indication of chlorophenol red sodium (the 1g/L WS)=1:1, and the change color of terminal point is for to become blue-green by yellow green;
Record V Titration, be calculated as follows the recovery of method;
Survey three parts of parallel appearance, calculate recovery rate and precision
。
6) 2,4, the purity testing of 5-triamido-6-hydroxy pyrimidine sulfate sample
Accurate 2 of 0.12 gram that takes by weighing in the beaker of 250mL; 4; 5-triamido-6-hydroxy pyrimidine sulfate sample is designated as
Figure 91437DEST_PATH_IMAGE003
, moves into the aforementioned HCl WS of having demarcated about 0.5mol/L of concentration of 25mL; And add 40mL distilled water, made it to dissolve in ultrasonic 5 minutes.Carry out titration with the aforementioned NaOH WS of having demarcated about 0.5mol/L of concentration, with pH BlankAs titration end-point;
Or the titration end-point indication changes bromcresol green sodium (the 1g/L WS) into by the acidometer indication: the acid mixture neutralization indicator indication of chlorophenol red sodium (the 1g/L WS)=1:1, and the change color of terminal point is for to become blue-green by yellow green;
Record V Titration, be calculated as follows sample purity;
Survey three parts of parallel appearance, calculate average purity and precision
。
The preferred compound concentration of the HCl WS in the step 1) is 0.5mol/L.
Step 2) the preferred compound concentration of the NaOH WS in is 0.5mol/L.
2,4, the general synthetic route of 5-triamido-6-hydroxy pyrimidine sulfate is suc as formula shown in 1:
Figure 897850DEST_PATH_IMAGE006
。
This target compound 2; 4; 5-triamido-6-hydroxy pyrimidine sulfate (suc as formula the compound 1 in 1) belongs to the aromatic primary amine compound of polyamino, and electron donating group is numerous on the aromatic rings, and its reactivity that generates diazo salt is relatively poor; Be prone to cause the mensuration result on the low side, so should not utilize diazo salt reaction the carrying out quantitative test of total primary amino radical.
Investigate 2,4, the general building-up process of 5-triamido-6-hydroxy pyrimidine sulfate (suc as formula the compound 1 in 1), its main accessory substance is a compound 4 and the sulfate of compound 2,3 and compound 2,3.Equal sulfur acid not in the compound 2,3,4; And the amino of compound 2,3 is few than compound 4; Its alkalescence is correspondingly than a little less than the compound 4; So its reaction with sulfuric acid can be as the compound 4 of triamido, according to the ratio generation acidic salt of 1:1, so the existence of impurity will cause its total acidity to reduce in the sulfate sample yet.Can adopt earlier and convert this sulfate to hydrochloride soluble in water, carry out the product quantitative test with the method for total acidity in the highly basic volumetric soiutions then.Through the recovery and the precision experimental test of method, its analysis result accurately and reliably.
Advantage of the present invention is:
1, adopt the Acid and Alkali Titration Analysis method, method is ripe, and is with low cost, easy and simple to handle.
2, adopt the macro-analysis method, the accuracy of method and precision are high.
Embodiment
Further set forth technical characterstic of the present invention below in conjunction with specific embodiment.
Embodiment 1
1, the preparation of the HCl WS of 0.5mol/L
Measure the dense HCl of 12mL with graduated cylinder, be dissolved in the 250mL distilled water, the HCl WS of preparation written treaty 0.5mol/L, to be calibrated.
2. the demarcation of the HCl WS of 0.5mol/L
(1) blank test
Use is measured the pH value of distilled water that obtain solution uses through the acidometer of straightened up in place, is designated as pH Blank, and as titration end-point.
(2) demarcation of HCl concentration of aqueous solution
Precision takes by weighing the anhydrous Na of about 0.5 gram 2CO 3, be designated as W NaCO3, place the beaker of 250mL, add the distilled water that 100mL had surveyed the pH value, ultrasonic dissolution.The HCl WS to prepare carries out titration, with pH BlankAs titration end-point, record V Titration(unit: mL), be calculated as follows the concentration C of the HCl WS HCl
Survey three parts of parallel appearance, average
Figure 714496DEST_PATH_IMAGE001
。
3. the preparation of the NaOH WS of 0.5mol/L
Take by weighing the NaOH of 5.0 grams, with the dissolved in distilled water of 250mL, to be calibrated.
4. the demarcation of the NaOH WS of 0.5mol/L
In the beaker of 250mL, accurately pipette the aforementioned HCl WS of having demarcated concentration of 10mL, add 100mL distilled water, carry out titration with the NaOH WS for preparing, with pH BlankAs titration end-point, record V Titration(unit: mL), be calculated as follows the concentration of the NaOH WS.
Survey three parts of parallel appearance, average
Figure 451508DEST_PATH_IMAGE002
。
5. the sulfate analytical approach is investigated
The precision and the recovery with this titrimetry of standard specimen test method.
Accurate 2 of 0.12 gram that takes by weighing in the beaker of 250mL; 4; 5-triamido-6-hydroxy pyrimidine sulfate standard specimen (purity 95%); Be designated as
Figure 787943DEST_PATH_IMAGE003
; Move into the aforementioned HCl WS of having demarcated about 0.5mol/L of concentration of 25mL, and add 40mL distilled water, made it to dissolve in ultrasonic 5 minutes.Carry out titration with the aforementioned NaOH WS of having demarcated about 0.5mol/L of concentration, with pH BlankAs titration end-point, record V Titration, be calculated as follows the recovery of method.
Survey three parts of parallel appearance, calculate recovery rate and precision
。
Average recovery rate through measuring this analytical approach is 100.0%, and relative average debiation is 0.11%.
6. 2,4, the purity testing of 5-triamido-6-hydroxy pyrimidine sulfate sample
Accurate 2 of 0.12 gram that takes by weighing in the beaker of 250mL; 4; 5-triamido-6-hydroxy pyrimidine sulfate sample is designated as
Figure 521730DEST_PATH_IMAGE003
, moves into the aforementioned HCl WS of having demarcated about 0.5mol/L of concentration of 25mL; And add 40mL distilled water, made it to dissolve in ultrasonic 5 minutes.Carry out titration with the aforementioned NaOH WS of having demarcated about 0.5mol/L of concentration, with pH BlankAs titration end-point, record V Titration, be calculated as follows sample purity.
Survey three parts of parallel appearance, calculate average purity and precision
Figure 2010102946607100002DEST_PATH_IMAGE007
。
By this method measure buied in present embodiment 2,4, the sample purity of 5-triamido-6-hydroxy pyrimidine sulfate is 93.46%, relative average debiation is 0.21%.
Embodiment 2
Just partly change the demarcation of HCl standard solution and NaOH standard solution into and adopt common acid neutralization indicator (like methyl orange and phenolphthalein) to carry out the titration end-point indication, all the other each several parts are identical with embodiment 1.By this method measure buied in present embodiment 2,4, the sample purity of 5-triamido-6-hydroxy pyrimidine sulfate is 93.56%, relative average debiation is 0.27%.
Embodiment 3
Partly change the demarcation of HCl standard solution and NaOH standard solution into employing common acid neutralization indicator (like methyl orange and phenolphthalein) and carry out the titration end-point indication; 2; 4; 5-triamido-standard specimen of 6-hydroxy pyrimidine sulfate and the indication of the titration end-point of sample change bromcresol green sodium (the 1g/L WS) into by the acidometer indication: the acid mixture neutralization indicator indication of chlorophenol red sodium (the 1g/L WS)=1:1, the change color of terminal point is for to become blue-green by yellow green.By this method measure buied in present embodiment 2,4, the sample purity of 5-triamido-6-hydroxy pyrimidine sulfate is 93.59%, relative average debiation is 0.52%.
The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.

Claims (1)

1. a titrimetry analyzes 2; 4; The method of 5-triamido-6-hydroxy pyrimidine sulfate sample purity is characterized in that: adopt and convert this sulfate to hydrochloride soluble in water earlier, carry out the product quantitative test with the method for total acidity in the highly basic volumetric soiutions then;
Its concrete steps are following:
1) the HCl WS of preparation 0.5 mol/L is to be calibrated;
2) the NaOH WS of preparation 0.5 mol/L is to be calibrated; Take by weighing the NaOH of 5.0 grams, with the dissolved in distilled water of 250mL, to be calibrated;
3) blank test
Use is measured the pH value of distilled water that obtain solution uses through the acidometer of straightened up in place, is designated as pH Blank, and as all titration end-points;
Or only in hydrochloric acid standard solution concentration calibration process, use at obtain solution to drip 1-2 in the distilled water and drip methyl orange indicator, become orange titration end-point of demarcating with HCl WS titration to the indicator color of above-mentioned preparation by yellow as hydrochloric acid;
Or only in NaOH concentration of standard solution calibration process; Use in the distilled water at obtain solution to drip 1-2 and drip phenolphthalein indicator, with step 2) said NaOH WS titration to the indicator color for preparing becomes the titration end-point that pink is demarcated as NaOH by colourless;
4) demarcation of HCl concentration of aqueous solution
Precision takes by weighing the anhydrous Na of 0.45-0.55 gram 2CO 3, be designated as
Figure FDA00001842201100011
Place the beaker of 250mL, add the above-mentioned distilled water of having surveyed the pH value of 100mL, ultrasonic dissolution carries out titration with the aforementioned HCl WS for preparing, with pH BlankAs titration end-point;
Or at this Na 2CO 3Drip 1-2 in the WS and drip methyl orange indicator, become orange by yellow as titration end-point with the color of methyl orange indicator;
Record V Titration, unit is mL, is calculated as follows the concentration C of the HCl WS HCl
Survey three parts of parallel appearance, average.
Figure FDA00001842201100021
5) demarcation of the NaOH WS of 0.5mol/L
In the beaker of 250mL, accurately pipette the aforementioned HCl WS of having demarcated concentration of 10mL, add 100mL distilled water, carry out titration with the NaOH WS for preparing, with pH BlankAs titration end-point;
Or in this HCl WS, drip 1-2 and drip phenolphthalein indicator, with the color of phenolphthalein indicator by the colourless pink that becomes as titration end-point;
Record V Titration, unit is mL, is calculated as follows the concentration of the NaOH WS;
Survey three parts of parallel appearance, average;
Figure FDA00001842201100022
6) this sulfate analytical approach is investigated
The precision and the recovery with this this titrimetry of sulfate standard specimen test method;
In the beaker of 250mL accurate take by weighing 0.12 gram purity be 95% 2,4,5-triamido-6-hydroxy pyrimidine sulfate standard specimen is designated as W Sulfate, move into the aforementioned HCl WS of having demarcated the 0.5mol/L of concentration of 25mL, and add 40mL distilled water, made it to dissolve in ultrasonic 5 minutes; Carry out titration with the aforementioned NaOH WS of having demarcated the 0.5mol/L of concentration, with pH BlankAs titration end-point;
Or the titration end-point indication changes bromcresol green sodium into by the acidometer indication: the acid mixture neutralization indicator indication of chlorophenol red sodium=1:1, and the change color of terminal point is for to become blue-green by yellow green; Described bromcresol green sodium and chlorophenol red sodium are the 1g/L WS;
Record V Titration, be calculated as follows the recovery of method;
Survey three parts of parallel appearance, calculate recovery rate and precision;
Figure FDA00001842201100031
7) 2,4, the purity testing of 5-triamido-6-hydroxy pyrimidine sulfate sample
Accurate 2,4 of 0.12 gram that takes by weighing in the beaker of 250mL, 5-triamido-6-hydroxy pyrimidine sulfate sample is designated as W Sulfate, move into the aforementioned HCl WS of having demarcated the 0.5mol/L of concentration of 25mL, and add 40mL distilled water, made it to dissolve in ultrasonic 5 minutes; Carry out titration with the aforementioned NaOH WS of having demarcated the 0.5mol/L of concentration, with pH BlankAs titration end-point;
Or the titration end-point indication changes bromcresol green sodium into by the acidometer indication: the acid mixture neutralization indicator indication of chlorophenol red sodium=1:1, and the change color of terminal point is for to become blue-green by yellow green; Described bromcresol green sodium and chlorophenol red sodium are the 1g/L WS;
Record V Titration, be calculated as follows sample purity;
Survey three parts of parallel appearance, calculate average purity and precision;
Figure FDA00001842201100032
。
CN2010102946607A 2010-09-28 2010-09-28 Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration Expired - Fee Related CN102141562B (en)

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CN104807953B (en) * 2015-05-26 2016-04-27 重庆长安汽车股份有限公司 A kind of method of quick detection oil dilution ratio
CN108375620A (en) * 2018-02-11 2018-08-07 南通市产品质量监督检验所 A kind of method that automatic potentiometric titration measures 2,4,5- triamido -6- hydroxy pyrimidine sulphates contents
CN110824101B (en) * 2019-11-14 2022-05-13 兰州蓝星纤维有限公司 Method for measuring functional groups on surface of carbon fiber

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