Reaction mass of propylidynetrimethanol and 2-ethylpropane-1,3-diol and 5-ethyl-1,3-dioxane-5-methanol

Hydrolysis

Link to relevant study record(s)

Reference

Endpoint:

hydrolysis

Type of information:

experimental study

Adequacy of study:

key study

Study period:

25 February 2010 - 2 March 2010

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: The study was conducted in accordance with OECD test guidelines, however no claim of GLP compliance was made, and a number of deviations from the guideline were recorded.

Qualifier:

according to guideline

Guideline:

OECD Guideline 111 (Hydrolysis as a Function of pH)

Deviations:

yes

Remarks:

no manual control of stable temperature and sterility

GLP compliance:

not specified

Remarks:

No information

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source (i.e. manufacturer or supplier) and lot/batch number of test material: 3577927 (lot no.)
- Purity, including information on contaminants, isomers, etc.: N/A

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: N/A
- Stability and homogeneity of the test material in the vehicle/solvent under test conditions (e.g. in the exposure medium) and during storage: N/A
- Stability in the medium, i.e. sensitivity of the test material to hydrolysis and/or photolysis: N/A
- Solubility and stability of the test material in the solvent/vehicle and the exposure medium: completely water soluble at 20 °C
- Reactivity of the test material with the incubation material used (e.g. plastic ware): N/A

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing (e.g. warming, grinding): N/A
- Preliminary purification step (if any): N/A
- Final concentration of a dissolved solid, stock liquid or gel: N/A
- Final preparation of a solid (e.g. stock crystals ground to fine powder using a mortar and pestle): N/A

FORM AS APPLIED IN THE TEST (if different from that of starting material)
- Specify the relevant form characteristics if different from those in the starting material, such as state of aggregation, shape of particles or particle size distribution: N/A

OTHER SPECIFICS
- Other relevant information needed for characterising the tested material, e.g. if radiolabelled, adjustment of pH, osmolality and precipitate in the culture medium to which the test chemical is added: log Pow: 0.2 (CTF); -0.2 (DMP); -0.8 (TMP).

Radiolabelling:

no

Analytical monitoring:

yes

Details on sampling:

- Sampling intervals for the parent/transformation products: Samples were analysed after 5 days' storage, for the parent compounds.
- Sampling method: Samples were allowed to reach room temperature then injected onto HPLC without dilution.
- Sampling methods for the volatile compounds, if any: N/A
- Sampling intervals/times for pH measurements: N/A
- Sampling intervals/times for sterility check: N/A
- Sample storage conditions before analysis: N/A
- Other observation, if any (e.g.: precipitation, color change etc.): N/A

Buffers:

- pH: 4±0.01 (20°C)
- Type and final molarity of buffer:
- Composition of buffer: citric acid/sodium hydroxide/hydrogen chloride

- pH: 7±0.01 (20°C)
- Type and final molarity of buffer:
- Composition of buffer: di-sodium hydrogen phosphate/potassium di-hydrogen phosphate

- pH: 9±0.01 (20°C)
- Type and final molarity of buffer:
- Composition of buffer: boric acid/potassium chloride/sodium hydrogen

Details on test conditions:

TEST SYSTEM
- Type, material and volume of test flasks, other equipment used: N/A
- Sterilisation method: N/A
- Lighting: N/A
- Measures taken to avoid photolytic effects: N/A
- Measures to exclude oxygen: N/A
- Details on test procedure for unstable compounds: N/A

TEST MEDIUM
- Volume used/treatment: N/A
- Kind and purity of water: N/A
- Preparation of test medium: N/A
- Renewal of test solution: N/A
- Identity and concentration of co-solvent: N/A

OTHER TEST CONDITIONS
- Adjustment of pH: pH was checked at the start and after 5 days
- Dissolved oxygen: N/A

Duration:

5 d

pH:

4

Temp.:

50 °C

Duration:

5 d

pH:

7

Temp.:

50 °C

Duration:

5 d

pH:

9

Temp.:

50 °C

Number of replicates:

Duplicate measurements at each pH.

Positive controls:

no

Negative controls:

no

Preliminary study:

A preliminary test was performed at 50°C and pH 4.0, 7.0 and 9.0.

Test performance:

No information.

Transformation products:

no

Remarks:

No significant levels of hydrolysis could be detected

Remarks on result:

not determinable

Remarks:

not applicable since Polyol TD is a mixture of several substances and only the major components were quantified.

Key result

pH:

4

Temp.:

50 °C

Remarks on result:

hydrolytically stable based on preliminary test

Key result

pH:

7

Temp.:

50 °C

Remarks on result:

hydrolytically stable based on preliminary test

Key result

pH:

9

Temp.:

50 °C

Remarks on result:

hydrolytically stable based on preliminary test

% Change in content of components:

(Difference found between sample stored at -20°C and +50°C after 5 days)

TMP:        pH 4 - 9.90%, 10.2%

pH 7 - -00.8%, -3.1%

pH 9 - 3.6%, 1.2%

DMP:        pH 4 - -0.8%, -1.9%

pH 7 - -5.0%, -4.1%

pH 9 - 0.5%, 1.1%

CTF:         pH 4 - 0.3%, 0.7%

pH 7 - 0.5%, -1.2%

pH 9 - 0.2%, -1.5%

Note that recovery values were not calculated as the test substance is a mixture of substances and only the major components were quantified.

Validity criteria fulfilled:

yes

Remarks:

- analysis of duplicate buffer solutions - test is repeatable and sensitive

Conclusions:

No sign of hydrolysis was seen under the conditions investigated.

Executive summary:

Hydrolyis of Polyol TD was studied in the dark at 50 °C in a heating cabinet in sterile aqueous buffered solutions at pH 4 (citric acid/ sodium hydroxide/ hydrogen chloride), pH 7 (di-sodium hydrogen phosphate/ potassium di.hydrogen phosphate) and pH 9 (boric acid/ potassium di-hydrogen phosphate) for 5 days.  At the end of the storage period, the samples at 50°C were analysed with samples which had been stored at -20°C, and the difference calculated. Samples were analysed by HPLC – refractive index detector at 0 and 5 days.

The experiment was conducted in accordance with the OECD test guideline 111. There is no information on GLP compliance.

It was concluded that no sign of hydrolysis was seen under the conditions investigated.

Description of key information

One study is available that studies the hydrolysis of Polyol TD at pH 4, 7 and 9.

Hydrolyis of Polyol TD was studied in the dark at 50 °C in a heating cabinet in sterile aqueous buffered solutions at pH 4 (citric acid/ sodium hydroxide/ hydrogen chloride), pH 7 (di-sodium hydrogen phosphate/ potassium di.hydrogen phosphate) and pH 9 (boric acid/ potassium di-hydrogen phosphate) for 5 days. Samples were analysed by HPLC – refractive index detector at 0 and 5 days.

It was concluded that no sign of hydrolysis was seen under the conditions investigated.

Additional information

All of the components in the Reaction mass of 2-ethylpropane-1,3-diol(DMP) and 5-ethyl-1,3-dioxane-5-methanol(CTF) and propylidynetrimethanol (TMP) are stable to hydrolysis i.e. the estimated half-life of the components is greater than one year under typical environmental conditions.