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Physical & Chemical properties

Water solubility

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Administrative data

Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
19 - 24 Nov 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Cross-reference
Reason / purpose:
reference to other study
Reference
Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
16 - 19 Nov 2018
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Remarks:
Preliminary study according to guidelines.
Reason / purpose:
reference to other study
Qualifier:
according to
Guideline:
OECD Guideline 105 (Water Solubility)
Version / remarks:
version July 27, 1995 / Preliminary test
Deviations:
no
GLP compliance:
no
Type of method:
other: preliminary test
Water solubility:
0.021 g/L
Temp.:
25 °C
pH:
>= 5 - <= 6

Specificity

The method proved to be specific; in fact it has been verified that blank, internal standard and matrix solutions do not interfere with the peaks of analyte.

 

Calibration

The calibration was tested on the active ingredient on 3 different concentration levels from 10 mg/L to 100mg/L of the theoretical amount of active ingredient in the water solution.

The calibration equation resulted: y = 16.926x - 0.0304 (R² = 1.00, R = 1.00).

The acceptance criteria (R > 0.99) was satisfied.

 

Preliminary test of Water solubility

The aqueous solubility in the Preliminary Test at 25 °C of the test item resulted as follows:

 

Preliminary test (visual)

Approximate solubility <1 g/L

-

Preliminary test (GC-MS analysis)

Aqueous solubility 0.021 g/L

RSD% = 17.15%

 

The pH determination of each test sample was estimated with a litmus paper, the result was between 5-6.

 

Conclusions

The preliminary test of water solubility of the test item was performed according to “OECD 105 Adopted by the Council on 27th July 1995”, by a GC-MS method.

The preliminary test, performed at 25 °C, proved that the water solubility is equal to 0.021 g/L.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2018

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 105 (Water Solubility)
Version / remarks:
Version July 27, 1995
Deviations:
no
GLP compliance:
no
Type of method:
flask method

Test material

Reference
Name:
Unnamed
Type:
Constituent

Results and discussion

Water solubility
Water solubility:
0.05 g/L
Temp.:
20 °C
pH:
>= 5.72 - <= 5.77

Any other information on results incl. tables

Selectivity

The GC/MS-SCAN Mode has proved itself as confirmatory technique.

 

Specificity

The method proved to be specific; in fact it has been verified that internal standard and matrix solutions do not interfere with the peak of chemical marker.

 

Linearity

Method Linearity was tested on 5 different concentration levels from 10 mg/L to 100 mg/L corresponding to range 20-200 % on the test sample solubility. All acceptance criteria (R > 0.99 and/or the confidence interval at 95% for the intercept contains zero) were satisfied.

 

Accuracy

Method accuracy was tested on reconstituted samples prepared at two concentration levels for chemical marker (LOQ and an high concentration, corresponding to 10 mg/L and 100 mg/L). The acceptance criterion (Recoveryactive ingredient= 70%-110%, and/or the confidence interval at 95% for the recovery contains 100%) proved to be satisfied.

 

Precision

The experimental RSD% respects the acceptance criteria. Six preparations for each concentration level were prepared but for the level at 100 mg/L, one preparation was discarded.

 

LOD and LOQ

LOD calculated as the chemical marker concentration with S/N ratio of 3 on the working standard solutions at LOQ level described in the Linearity paragraph and on reconstituted sample at 10 mg/L. The LOQ is defined as the concentration at which all acceptance criteria of this study are met. The LOQ is the chemical marker concentration at which the S/N ratio is at least 10 and corresponds to the lowest validated level.

 

LOD (mg/L) calculated

S/N ~ 3

0.07

LOQ (mg/L) calculated

S/N ~ 10

0.22

LOQ (mg/L) validated

This concentration met all acceptability criteria

10

 

 

Water solubility test

The aqueous solubility at 20 °C of the test item is reported in the following table.

 

Water solubility test

Aqueous solubility = 0.050 g/L

RSD% = 3.52

 

The results from vessels 1 to 3 appeared constant and their RSD% did not differ by more than 15%. For this reason the results of these three first flasks, are averaged.

 

The pH determination at 20 °C of each test sample are reported in the following table.

 

S1

S2

S3

pH (20°C)

5.77

5.74

5.72

Conclusions

The water solubility of test item was performed according to “OECD 105 Adopted by the Council on 27th July 1995” by an GC/MS method.

Parameters verified during this analytical method, developed and validated according to SANCO/3030/99 rev.4, were: Specificity, Linearity, Accuracy, Precision and LOD/LOQ.

The method proved to be specific, linear, precise and accurate.

The aqueous solubility at 20 °C proved to be equal to 0.050 g/L

Applicant's summary and conclusion