Reaction mass of [3R-(3α,3aβ,6α,7β,8aα)]-octahydro-3,6,8,8-tetramethyl-1H-3a,7-methanoazulen-6-ol and [3R-(3α,3aβ,6α,7β,8aα)]-octahydro-3,6,8,8-tetramethyl-1H-3a,7-methanoazulen-5-yl acetate

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Guideline study performed under GLP. All relevant validity criteria were met.

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

Principles of method if other than guideline:

Determination of the water solubility of the test item employing of the study the column elution method (OECD TG 105, 1995). The test item is eluted with water from a micro column which is charged with an inert support material, previously coated with an excess of the test item. The water solubility is given by the mass concentration of the eluate when this has reached a plateau as a function of time. The decision of the column elution method was made due to the test item properties: low soluble (< 10 mg/L expected) liquid substance and based on the results of preliminary testing using each of the guideline methods (non-GLP). The preliminary test was using the definitive test column elution methodology, but without temperature monitoring as a rangefinder with a total of four samplings on two sampling dates. Care was taken to ensure sufficient test item resevoir and/or demonstration of equilibrium having been reached for the measured constituents during preliminary testing and prior to definitive testing.

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected June 2013; signature: February 2016

Type of method:

column elution method

Water solubility:

3.52 mg/L

Temp.:

20 °C

pH:

7

Remarks on result:

other: Constituent 1; pH 7.0

Water solubility:

0.691 mg/L

Temp.:

20 °C

pH:

7

Remarks on result:

other: Constituent 2; pH 7.0

Preliminary test:

The result was a water solubility of 0.755 mg/L for constituent 1 as well as 3.36 mg/L for constituent 2.

 

Definitive test:

The solubility of the test item in double distilled water was determined employing the column elution approach at 20 ± 0.5 °C with The micro column was equilibration overnight and experimental determination at 20 ± 0.5 °C. The water solubility was respectively at pH 7:

3.52 mg/L (constituent 1);

0.69 mg/L (constituent 2) and

The test item concentration of five consecutive fractions was constant within 30% for both flow rates and both analytes and the mean values obtained from two tests with different flow rates did not differ by more than 30% for both analytes. The analytical method (GC MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity according to SANCO 3029/99 rev 4.

Conclusions:

Interpretation of results: slightly soluble (0.1-100 mg/L)The test substance water solubility was determined to be 3.52 mg/L (constituent 1); 0.691 mg/L (constituent 2) of solution at pH 7 and 20.0 °C. The test substance occupies the 'slightly soluble' (0.1-100 mg/L) solubility band based on measurements of two main constituents.

Executive summary:

The water solubility of the substance was determined according to OECD Method 105 and EU Method A.6 column elution method. Based on the results of preliminary and definitive testing equilibrium was reached for the main constituents. The test item was passed through the equilibrated micro column and samples were separated by time intervals of at least ten bed volumes (15 min at 0.4 mL/min), were taken and analyzed as until five successive samples did show concentrations did not show concentrations differing by more than ± 30% in a random fashion. A second run was performed at half the flow rate (0.2 mL/min) of the first test. As the result of the second run confirms that of the first test, the test was concluded. The analytical method (GC MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. The test item concentrations of at least five consecutive fractions were constant within 30% and the mean values obtained from two tests with different flow rates did not differ for more than 30%. The mean water solubility of the substance was determined to be 3.52 mg/L (constituent 1) and 0.691 mg/L (constituent 2) of solution at pH 7 and 20 ± 0.5 °C.

Description of key information

Water Solubility: 3.52 mg/L (constituent 1); 0.691 mg/L (constituent 2) at pH 7 and 20 ± 0.5 °C, OECD TG 105 column elution method, 2016

Additional information

The water solubility of the substance was determined according to OECD Method 105 and EU Method A.6 column elution method. Based on the results of preliminary and definitive testing equilibrium was reached for the main constituents. The test item was passed through the equilibrated micro column and samples were separated by time intervals of at least ten bed volumes (15 min at 0.4 mL/min), were taken and analyzed as until five successive samples did show concentrations did not show concentrations differing by more than ± 30% in a random fashion. A second run was performed at half the flow rate (0.2 mL/min) of the first test. As the result of the second run confirms that of the first test, the test was concluded. The analytical method (GC MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. The test item concentrations of at least five consecutive fractions were constant within 30% and the mean values obtained from two tests with different flow rates did not differ for more than 30%. The mean water solubility of the substance was determined to be 3.52 mg/L (constituent 1) and 0.691 mg/L (constituent 2) of solution at pH 7 and 20 ± 0.5 °C.