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Physical & Chemical properties

Additional physico-chemical information

Administrative data

Endpoint:
other: analytical method
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From 24 August 2015 to 06 November 2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Study performed according to recognized international guideline and under GLP.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2015
Report date:
2015

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
other: SANCO/3030/99 rev. 4 from 11/07/00
Deviations:
no
GLP compliance:
yes (incl. QA statement)

Test material

Constituent 1
Reference substance name:
hydrogen sulfate;tetrakis(hydroxymethyl)phosphanium;urea
EC Number:
613-239-6
Cas Number:
63502-25-0
Molecular formula:
Not applicable
IUPAC Name:
hydrogen sulfate;tetrakis(hydroxymethyl)phosphanium;urea
Constituent 2
Reference substance name:
Phosphonium, tetrakis (hydroxymethyl)- sulphate(2:1); polymer with urea
IUPAC Name:
Phosphonium, tetrakis (hydroxymethyl)- sulphate(2:1); polymer with urea
Test material form:
other: dried sample
Details on test material:
- Name of test material (as cited in study report): Phosphonium, tetrakis (hydroxymethyl)-sulphate(2:1); polymer with urea
For others details see the section Confidential details on test material

Results and discussion

Results:
The analytical method shows a good specificity for Active Ingredients analysis.
The relation between the quantity of Active Ingredients and the equivalent volume of iodine is linear within the range of 19.47 to 142.88 mg of Active Ingredients.
The accuracy results of Active Ingredients are in conformity with the Guidelines requirements. Indeed, the recovery results should be in the range 98-102% and they are experimentally between 99.3% and 100.3%
The concentration of Active Ingredients in the test item was equal to 94.0% w/w or 940 g/kg. In the case of Active Ingredients, the precision was acceptable as the R.S.D was lower than the results of the modified Horwitz equation (0.54%< 1.35%).
The limit of detection (LOD) of Active Ingredients was defined as 1.64 mg of Active Ingredients.
The limit of quantification (LOQ) of Active Ingredients was defined as 4.98 mg of Active Ingredients.

Any other information on results incl. tables

Specificity:

In the test item and in the reference item, the initial solution is colorless and become dark/purple at the point of equivalence. Nearly the same volume of 0.05N iodine solution is necessary to reach the point of equivalence in both items.

In the solvent blank the initial solution was colorless. After addition of 0.1 mL of the 0.05 iodine solution, a coloration dark/purple was observed. As this volume of 0.1 mL is lower (<1%) of the volume required to reach the point of equivalence in the test items, the specificity was defined.

Additionally, no interferences of the detection and quantification of Active Ingredients in the test item solutions is observed.

Linearity:

The correlation coefficient of the calibration curve obtained by the analysis of 5 test item solutions is: r² = 0.9999.

The concentration of the test item solutions used for the calibration curve are between 19.47 and 142.88 mg.

Accuracy:

The recovery rates of Active Ingredients in the two spiked solutions of test item are between 99.3 and 100.3%.

Precision:

The mean content of the five analysed test item solutions is 94.0% (w/w).

The standard deviation related to the mean content is 0.5% (w/w) and the Relative Standard Deviation (RSD) is 0.54%.

The modified Horwitz equation is verified. Indeed :

R.S.D < 2(1 -0.5*log C)*0.67

0.54 < 2(1 -0.5*log 0.94)*0.67

0.54 < 1.35

According to the guideline requirement, the precision of the analytical method is therefore considered to be fulfilled.

Limit of detection (LOD) and limit of quantification (LOQ):

The limit of detection (LOD) and the limit of quantification (LOQ) are defined through the regression curve.

Mass (mg)
LOD 1,64 of active ingredients
LOQ 4,98 of active ingredients

Applicant's summary and conclusion

Conclusions:
The analytical method is validated for the test item between 19.47 and 142.88 mg of Active Ingredients in water.
Executive summary:

The validation of an analytical method (titration method) for the determination of Active Ingredients in dried extract of Phosphonium, tetrakis (hydroxymethyl)-sulphate(2:1); polymer with urea will be done in compliance with the SANCO/3030/99 rev.4. No deviation from the guideline was observed in this GLP study.

The analytical method is validated by definition of the specificity, the linearity, the accuracy, the precision and the limit of detection and the limit of quantification of the method.

The analytical method shows a good specificity for Active Ingredients analysis.

The relation between the quantity of Active Ingredients and the equivalent volume of iodine is linear within the range of 19.47 to 142.88 mg of Active Ingredients.

The accuracy results of Active Ingredients are in conformity with the Guidelines requirements. Indeed, the recovery results should be in the range 98-102% and they are experimentally between 99.3% and 100.3%

The concentration of Active Ingredients in the test item was equal to 94.0% w/w or 940 g/kg. In the case of Active Ingredients, the precision was acceptable as the R.S.D was lower than the results of the modified Horwitz equation (0.54%< 1.35%).

The limit of detection (LOD) of Active Ingredients was defined as 1.64 mg of Active Ingredients.

The limit of quantification (LOQ) of Active Ingredients was defined as 4.98 mg of Active Ingredients.

The analytical method is validated for the test item between 19.47 and 142.88 mg of Active Ingredients in water.

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