(+-)-(3aRS,5aSR,9aSR,9bSR)-3a,6,6,9a-Tetramethyldodecahydronaphtho[2,1-b]furan

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Experimental phase from 2014-03-17 to 2014-12-22

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

The study was conducted according to an internationally recognised method, and under GLP. No relevant deviation was reported. Test substance is adequately specified. Therefore full validation applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

yes

Remarks:

excess test item

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

yes

Remarks:

excess test item

Principles of method if other than guideline:

Testing was conducted in both double distilled water and daphnia reconstituted natural medium M4 (OECD 211).

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected on June 3 to 5, 2013 / signed on November 5, 2013

Type of method:

flask method

Remarks:

modified acc. to Letinski et al. (2002) and OECD 123

Specific details on test material used for the study:

Storage condition of test material: Room temperature, protected from light, in the original container (aluminium bottle)

Key result

Water solubility:

10.2 mg/L

Conc. based on:

test mat.

Loading of aqueous phase:

0.1 other: %vol

Temp.:

20 °C

pH:

7

Remarks on result:

other: in double distilled water

Water solubility:

9.9 mg/L

Temp.:

20 °C

pH:

7

Remarks on result:

other: in daphnia medium (M4)

Details on results:

The analytical method was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity:
LOD = 0.01 mg/L
System quantification limit = 0.05 mg/L
Linearity: 0.05 – 1 mg/L (n = 6), r2 ranging between 0.9983 and 0.9996
LOQ (target): nominal 0.2 mg/L
Recovery rates in double distilled water:
1 x LOQ = 87% (RSD=3.9%)
3 x LOQ = 82% (RSD=3.7%)
Recovery rates in daphnia M4 medium:
1 x LOQ = 85% (RSD=2.6%)
3 x LOQ = 83% (RSD=3.6%)
Specificity: Response of blank values was significantly lower than 30 % of LOQ, actually no signal higher than the background was observed.

Preliminary Test

The determined solubility was 9.22 mg/L for double distilled water and 8.18 mg/L for daphnia medium for the centrifuged samples. The results obtained with un‑centrifuged samples vary between 11,6 mg/L and 425 mg/L. As the un‑centrifuged samples were not obtained under slow‑stirring conditions, their results were not further taken into account. Due to technical reasons (facilitating the handling), 0.1 % v/v (approx. 1 g/L) was used for the application dose in the definitive test.

Water solubility results

For each sample, no Tyndall‑effects were observed. (6 sampling time, 2 media, un-centrifuged and centrifuged)

Equilibrium was considered reached from 43h after temperature reduction.

The solubility of the test item in double distilled water and daphnia M4 medium was determined for un‑centrifuged and centrifuged samples, respectively (average of 6 consecutive sampling x 2 replicates):

Water solubility [mg/L] ± SD
Test medium		Uncentrifuged	Centrifuged
Double distilled water		10.2 ± 0.4	4.4 ± 1.4
Daphnia M4 medium		9.9 ± 0.5	4.3 ± 1.6

Conclusions:

Interpretation of results (migrated information): slightly soluble (0.1-100 mg/L)

Executive summary:

The water solubility of the test item was determined under GLP, according to OECD 105 / EU A6 guideline, using the flask method with slow-stirring approach, in double distilled water and daphnia medium M4, at 20 ± 0.5 °C with 72h preincubation at 30 ± 0.5 °C . Duplicate test vessels were prepared.

Analytical evaluation was performed with GC-MS using the test item for external calibration. The method was validated with satisfactory results regarding linearity, limit of quantification, accuracy, precision and specificity.

Equilibrium was considered achieved 43h after reduction to test temperature.

The pH-values were measured with indicator strips. All samples were checked negative for colloidal dispersed material utilising the Tyndall effect.

The water solubility (20 °C, pH 7) was determined to be 10.2 mg/L in distilled water, and 9.9 mg/L in daphnia medium M4.

Description of key information

Slightly soluble. Equilibrium reached from 43 hours.

pH of saturated solution: 7

Key value for chemical safety assessment

Water solubility:

10.2 mg/L

at the temperature of:

20 °C

Additional information

A fully reliable experimental study, conducted according to a recognized OECD/EC method and under GLP, is available. Therefore, it is considered as a key study, and the result is retained as key data.