Registration Dossier

Administrative data

Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
01/02/2017 – 23/02/2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2017
Report Date:
2017

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
EU Method A.6 (Water Solubility)
Version / remarks:
EU Regulation (EC) 440/2008, Annex Part A test A6
Qualifier:
according to
Guideline:
OECD Guideline 105 (Water Solubility)
GLP compliance:
yes (incl. certificate)
Other quality assurance:
other: QA SOP 010
Remarks:
The procedure of the determination of whether the study live phase is audited by the QA unit is set out in QA SOP 010 and is determined at the time the QA unit receives study notification.
Type of method:
flask method

Test material

Reference
Name:
Unnamed
Test material form:
solid
Details on test material:
- Stabilisation: stable
- Safety precautions: The routine hygienic procedures were sufficient to assure personnel health and safety
- Colour: brownish red
- Storage conditions: room temperature

Results and discussion

Water solubility
Key result
Water solubility:
2.067 g/L
Temp.:
20 °C
pH:
6.67

Any other information on results incl. tables

The peak area of the di-sulfonic acid (Retention time approximately 4.2 minutes) was used for the water solubility determination. The analysis was carried out with duplicate injections of samples prepared from each flask and the corresponding mean peak area calculated.

As the test sample was also used for the calibration, an assumption was made that all components present had the same extinction coefficient and no undetectable components were present. The purity for the product was taken as the mean of six replicates prepared at the 100% level of the calibration.

It was noted that after the shaking period only a small amount of sample remained undissolved in the flask. As a consequence a second set of test samples were prepared at a concentration of 12 g/L. Analysis of the 12 g/L samples gave inconsistent and lower results (Day 1 - 1.72 g/L, Day 2 – 1.19 g/L and Day 3 - 1.21 g/L) than those obtained for the samples prepared at 2.5 g/L. The implication being that at varying sample concentrations, the chromatographic profile changes. The change in chromatographic profile may be due to the multicomponent nature of the product.

Applicant's summary and conclusion

Conclusions:
Mean water solubility (gL-1): 2.067
Executive summary:

Comment:

The peak area of the di-sulfonic acid (Retention time approximately 4.2 minutes) was used for the water solubility determination. The analysis was carried out with duplicate injections of samples prepared from each flask and the corresponding mean peak area calculated.

As the test sample was also used for the calibration, an assumption was made that all components present had the same extinction coefficient and no undetectable components were present. The purity for the product was taken as the mean of six replicates prepared at the 100% level of the calibration.

It was noted that after the shaking period only a small amount of sample remained undissolved in the flask. As a consequence a second set of test samples were prepared at a concentration of 12 g/L. Analysis of the 12 g/L samples gave inconsistent and lower results (Day 1 - 1.72 g/L, Day 2 – 1.19 g/L and Day 3 - 1.21 g/L) than those obtained for the samples prepared at 2.5 g/L. The implication being that at varying sample concentrations, the chromatographic profile changes. The change in chromatographic profile may be due to the multicomponent nature of the product.