α-(2,4-dichlorophenyl)-1H-imidazole-1-ethanol

Hydrolysis

Link to relevant study record(s)

Reference

Endpoint:

hydrolysis

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-05-23 to 2017-05-30

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 111 (Hydrolysis as a Function of pH)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method C.7 (Degradation: Abiotic Degradation: Hydrolysis as a Function of pH)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 835.2120 (Hydrolysis of Parent and Degradates as a Function of pH at 25°C)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material:
* Identification: JNJ-123955-AAA (T000824)
* Batch: M15KB5305
* Test item number: 207720/B
- Expiration date of the lot/batch: 2019-11-24 (retest date)
- Purity test date: 2016-10-21 (certificate of analysis release date)

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability under test conditions: no data

Analytical monitoring:

yes

Details on sampling:

- Sampling intervals for the parent/transformation products:
* Tier 1: at the beginning and after 5 days.

- Sampling method:
* Tier 1: Concentration of the test item in the test sample was determined immediately after preparation. The samples taken at t=5 days were cooled to room temperature using running tap water. The samples were diluted in a 4:1 (v:v) ratio with acetonitrile and analysed.

Buffers:

- pH:
* Tier 1: 4.0, 7.0, and 9.0

- Type, final molarity and composition of buffer:
* acetate buffer pH 4: solution of 16.7% 0.1 M sodium acetate in water and 83.3% 0.1 M acetic acid in water. The buffer contains 0.0009% (w/v) sodium azide.
* Phosphate buffer pH 7: solution of 0.1 M potassium di-hydrogenphosphate in water adjusted to pH 7 using 10N sodium hydroxide. The buffer contains 0.0009% (w/v) sodium azide.
* Borate buffer pH 9: solution of 0.1 M boric acid in water and 0.1 M potassium chloride in water adjusted to pH 9 using 1N sodium hydroxide. The buffer contains 0.0009% (w/v) sodium azide.

Details on test conditions:

TEST SYSTEM
- Type, material and volume of test flasks, other equipment used: sterile vessel
- Sterilisation method: buffer solutions were filter-sterilised through a 0.2 µm FP 30/0.2 CA-S filter (Wathman, Dassel, Germany) and transferred into a sterile vessel.
- Lighting: in the dark
- Measures taken to avoid photolytic effects: vessels placed in the dark
- Measures to exclude oxygen: nitrogen gas was purged through the solution for 5 minutes
- Details on test procedure for unstable compounds: no data
- Details of traps for volatile, if any: not applicable
- If no traps were used, is the test system closed/open: under vacuum
- Is there any indication of the test material adsorbing to the walls of the test apparatus? no

TEST MEDIUM
- Volume used/treatment: 6 mL
- Kind and purity of water: Milli-Q
- Preparation of test medium: The test item was spiked to the solutions at a target concentration of 9 mg/L using a spiking solution in acetonitrile.
- Renewal of test solution: not applicable
- Identity and concentration of co-solvent: not applicable

OTHER TEST CONDITIONS
- Adjustment of pH: no
- Dissolved oxygen: no data

Duration:

5 d

pH:

4

Temp.:

49.3 °C

Initial conc. measured:

9.21 mg/L

Duration:

5 d

pH:

4

Temp.:

49.3 °C

Initial conc. measured:

9.24 mg/L

Duration:

5 d

pH:

7

Temp.:

49.3 °C

Initial conc. measured:

9.61 mg/L

Duration:

5 d

pH:

7

Temp.:

49.3 °C

Initial conc. measured:

9.56 mg/L

Duration:

5 d

pH:

9

Temp.:

49.3 °C

Initial conc. measured:

9.24 mg/L

Duration:

5 d

pH:

9

Temp.:

49.3

Initial conc. measured:

9.22 mg/L

Number of replicates:

2

Positive controls:

no

Negative controls:

no

Statistical methods:

no data

Preliminary study:

The preliminary hydrolysis tests were performed at 49.3°C +/- 0.7°C. At pH 4, pH 7 and pH 9 a degree of hydrolysis of < 10% was observed after 5 days. It demonstrated that the half-life time of the test item at 25°C is > 1 year. According to the guideline, no further tests were required.

Transformation products:

no

% Recovery:

103

pH:

4

Temp.:

49.3 °C

Duration:

5 d

Remarks on result:

hydrolytically stable based on preliminary test

Remarks:

103% and 102% for each replicates

% Recovery:

107

pH:

7

Temp.:

49.3 °C

Duration:

5 d

Remarks on result:

hydrolytically stable based on preliminary test

Remarks:

106% and 107% for each replicates

% Recovery:

103

pH:

9

Temp.:

49.3 °C

Duration:

5 d

Remarks on result:

hydrolytically stable based on preliminary test

Remarks:

103% and 102% for each replicates

Key result

pH:

4

Temp.:

25 °C

DT50:

> 1 yr

Key result

pH:

7

Temp.:

25 °C

DT50:

> 1 yr

Key result

pH:

9

Temp.:

25 °C

DT50:

> 1 yr

Validity criteria fulfilled:

yes

Remarks:

No test item was detected in the blank buffer solutions. The mean recoveries of the buffer solutions fell within the criterion range of 90-110%. It demonstrated that the analytical method was adequate to support the hydrolysis study on the test item.

Conclusions:

T000824 was found to be hydrolytically stable at pH 4.0, pH 7.0 and pH 9.0 with a degree of hydrolysis of < 10% after 5 days. It demonstrated that the half-life time of the test item at 25°C is > 1 year and the test item was considered hydrolytically stable. Therefore, no further testing was performed. The results of the test can be considered reliable without restriction.

Description of key information

One study (Ciric, 2017) was performed according to OECD guideline 111 and regarded as a key study (Klimisch score of 1). A half-life time of > 1 year at 25 °C and pH 7 was determined for T000824.