N-[[3,5-dichloro-2-fluoro-4-(1,1,2,3,3,3-hexafluoropropoxy)phenyl]carbamoyl]-2,6-difluorobenzamide

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

31 July 2000 - 09 August 2000

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Study conducted in compliance with agreed protocols, with no or minor deviations from the standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of the relevant results. The study report was conclusive, done to valid guidelines and conducted under GLP conditions.

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7840 (Water Solubility)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

GLP compliance:

yes

Type of method:

column elution method

Key result

Water solubility:

0.194 mg/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

>= 6.18 - <= 6.65

Remarks on result:

other: ± 0.025 mg/L

Details on results:

Preliminary Study:
A preliminary study was not conducted since a molecule similar to the test material indicated a solubility of > 10 E-03 g/L, which is the upper recommended range for the column elution method.

Method Evaluation:
The spiked units from two separate stock solutions were found to have recovery values of 103 and 96.8 %, confirming the effectiveness of the method.
The five working standard solutions, prepared from separate stock solutions, indicated that the samples were assayed in a linear range for the method.
The method ws determined to be suitable to assay the units within the working range based on the correlation coefficient.

Solubility determination:
The solubility results can be seen in Table 2. The relative difference between each replicate was less than 30 %, confirming that the solubility values reflected an equilibrium of saturated solutions.
The fractions collected from the 6 mL/hr flow rate were not required.
No bias from pH solutions was observed, see Table 3.
Contents of vials were inspected to determine if a ‘Tyndall’ effect occurred as light passed through the solution. No discolouration was observed. Neither cloudiness nor particulate matter was observed.
The representative calibration curve from standards of the test material showed linearity of the curve with a correlation coefficient (r) of 0.9984474.

Table 2: Solubility in Unbuffered Water

Sample ID*	Concentration (ng/mL)	Average (ng/mL)	SD (n=5)
V7:12	166	194	28
V8:12	221
V9:12	196
V10:12	223
V11:12	164
V7:25	189	193	23
V8:25	214
V9:25	157
V10:25	231
V11:25	189

*Vial:Elution Flow (mL/hr)

Table 3: pH values

Sample ID*	pH
Initial unbuffered water	6.65
V6:12	6.18
V12:12	6.23
V6:25	6.23
V12:25	6.25

*Vial:Elution Flow (mL/hr)

Conclusions:

Interpretation of results: slightly soluble (0.1-100 mg/L)
Under the conditions of the test, the solubility of the test material was determined to be 0.194 ± 0.025 mg/L at 20 ± 0.5 °C.

Executive summary:

The water solubility of the test material was determined using the column elution method in a GLP study conducted in accordance with the standardised guidelines EPA OPPTS 830.7840 and OECD 105.

The water solubility was determined in unbuffered at 20 ± 0.5 °C. Saturated aqueous sampled were prepared by elution of unbuffered water through a column packed with an inert support, coated with the test material. The water was eluted through the column at two flow rates, 25 mL/hr and 12 mL/hr. Replicate samples were assayed by HLPLC and an average concentration was determined for each flow rate. The two solubility values were averaged, and the solubility value for each flow rate was within 30 % of the average. An external calibration curve was prepared by analysing standard solution of the test material and the concentrations of the samples were determined from the calibration curve.

Under the conditions of the test, the solubility of the test material was determined to be 0.194 ± 0.025 mg/L at 20 °C.

Description of key information

Water solubility 0.194 mg/L at 20 °C, column elution method, EPA OPPTS 830.7840, OECD 105, Busse 2000.

Key value for chemical safety assessment

Water solubility:

0.194 mg/L

at the temperature of:

20 °C

Additional information

The water solubility of the test material was determined using the column elution method in a GLP study conducted in accordance with the standardised guidelines EPA OPPTS 830.7840 and OECD 105. The study was assigned a reliability score of 1, reliable without restrictions, in line with the principles of Klimisch et al. (1997).

The water solubility was determined in unbuffered at 20 ± 0.5 °C. Saturated aqueous sampled were prepared by elution of unbuffered water through a column packed with an inert support, coated with the test material. The water was eluted through the column at two flow rates, 25 mL/hr and 12 mL/hr. Replicate samples were assayed by HLPLC and an average concentration was determined for each flow rate. The two solubility values were averaged, and the solubility value for each flow rate was within 30 % of the average. An external calibration curve was prepared by analysing standard solution of the test material and the concentrations of the samples were determined from the calibration curve.

Under the conditions of the test, the solubility of the test material was determined to be 0.194 ± 0.025 mg/L at 20 °C.