Reaction products of neodecanoic acid and titanium (IV) isopropoxide

Long-term toxicity to fish

Administrative data

Endpoint:

adult fish: sub(lethal) effects

Type of information:

experimental study

Adequacy of study:

key study

Study period:

The study was conducted between 11 August 2011 and 31 August 2011

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted to GLP and in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not effect the quality of the relevant results.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2011

Report date:

2011

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 204 (Fish, Prolonged Toxicity Test: 14-day Study)

Deviations:

no

GLP compliance:

yes

Test material

Test material information

Constituent 1

Reference substance name:

E0286P/040A

IUPAC Name:

E0286P/040A

Details on test material:

Product name: E0286P/040A
CAS No.: not supplied
Appearance: yellow liquid
Purity: 100%
Water solubility: insoluble
Stability: stable
Vapor Pressure: not supplied
Relative density: 990 kg/m3 (0.99g/cm3) at 20°C
Lot number: E0286P/040A/01
Expiry date: 12/30/2011
Storage: keep container closed in a room temperature (15-25°C).

Specific details on test material used for the study:

Details on properties of test surrogate or analogue material (migrated information):
None

Sampling and analysis

Analytical monitoring:

yes

Details on sampling:

Verification of Test Concentration

Determination of total organic carbon (TOC):
The concentration of total organic carbon (TOC) was determined in samples of test media. Samples were taken from each test vessel and analyzed in the fresh media at 0-day, 7-day and 13-day, and in the expired media at 1-day, 8-day and 14-day.

Chemical analysis for concentration of neodecanoic acid in test samples:
The concentration of neodecanoic acid in the test media was determined by reverse-phase high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Samples were taken from each test vessel and analyzed in the fresh media at 0-day, 7-day and 13-day, and in the expired media at 1-day, 8-day and 14-day.

Test solutions

Vehicle:

no

Details on test solutions:

Exposure Concentration and Grouping:
Based on the preliminary test, a 'limit test' was performed at 100 mg/L as WAF. A concurrent control group was performed in parallel. 10 fish were used in both the test concentration and the control groups.

Preparation of Test Solution
The Water Accommodated Fraction (WAF) was formulated for the test concentration by combining the test item and dilution water on a weight to volume basis. WAFs were prepared separately for the test concentration approximately 24 hours prior to the start of the test and each media renewal period. Glass jars (diameter: 20cm, high: 40 em, with water ca 10 liters) were used to stir the WAF solutions.

A measured weight of test item obtained using the decreasing method, was added to a measured volume of test medium. For this test item, a syringe was used .to dispense it onto the surface of the water. The method of adding the test item to the water was as follows: 1) first weighed a syringe, 2) then took about 1.0 ml of the test item with the syringe and weighed, 3) dispensed the test item onto the surface of the water, 4) weighed the syringe and residual test item, 5) calculated the weight of test item which was added to 10 liters of test water. During the study period, the weight of test item was between 0.9191g tol.0358 g.

The test item/dilution water combinations were stirred at test temperature (22.9-23.9°C) for 22 hours according to the equilibrating time. Stirring was accomplished by using a magnetic mixer and adjusting the mixer speed such as a vortex was formed which represented a slight dimple at the water surface. Following the mixing period, the formulations was allowed to settle for 2 hour.

Upon completion of the WAF mixing and settling period, the aqueous solution was drained from below the surface of preparation vessel. The first 5 to 10 mL of solution decanted from the vessel was discarded. The remaining solution was used undiluted in the exposure vessels.

After intervals of 24 hours the fish were transferred to different tanks containing freshly prepared solutions during the fourteen days-test period.

Test organisms

Test organisms (species):

Danio rerio (previous name: Brachydanio rerio)

Details on test organisms:

Selection of Species:
Zebra fish is the preferred species for this study recommended by the Guidelines for the Testing of Chemicals (2004), Environmental Protection Agency of People's Republic of China, and is one of the recommended species ofthe OECD Guidelines for the Testing of Chemicals. The batch used for this definitive test was zebra fish/20110517.

Acclimation
Fish were held in the laboratory for more than 12 days to acclimatize to the test conditions. No effects or deaths were found during the acclimation period.

Study design

Test type:

semi-static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

14 d

Post exposure observation period:

Obersvations:
Total lengths and wet weights of the fish used in treated and control groups were measured at the start and end of the test period.
During the test, the fish in treated and control groups were inspected daily for mortality and toxic signs.

Physicochemical Measurements:
Dissolved oxygen, pH and water temperature were measured at 0-day, 7-day, and 13-day for the fresh and expired solutions during the 14-day exposure period.

Euthanasia of tested fish
After 14 days of exposure, all of the surviving fish were euthanatized. The method of euthanasia was to put the fish into 0.2-0.5% water solution of Ethylene Glycol Monophenyl Ether. After 5 to 15 seconds, the fish were dead.

Test conditions

Hardness:

The hardness was aprox. 240 mg/L (as CaC03).

Test temperature:

Temperature: 23±2 °C.

pH:

The ranges for pH was 7.14 to 7.93. The acceptable (or recommended) range for pH value is 6.0 to 8.5, throughout the test.

Dissolved oxygen:

The ranges for dissolved oxygen was 6.05 to 8.23mg/L. The acceptable (or recommended) range for dissolved oxygen is at least 5.8mg/L throughout the test.

Salinity:

Not applicable

Nominal and measured concentrations:

Based on the results of the preliminary test, a definitive test was conducted using a limit test concentration of 100 mg/L, as Water Accommodated Fraction (WAF) (nominal concentration). A concurrent water control group was performed in parallel. The definitive test was performed with a semi-static water renewal system and the water used was reconstituted water (ISO 6341-1982).

Details on test conditions:

Conditions of exposure:

Semi-static test: the test was performed with renewal of the test solutions every 24 hours.
Duration: 14 days;
Loading: less than 1.0 g fish/liter water;
Light: 12 hours photoperiod daily;
Temperature: 23±2 °C;
Oxygen concentration: not less than 60% of ASV during the test period;
Feeding: daily (the quantity offood being kept constant).

Reference substance (positive control):

no

Results and discussion

Effect concentrations

Duration:

14 d

Dose descriptor:

NOEC

Effect conc.:

100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mortality

Remarks on result:

other: CL not stated

Details on results:

Physiocochemical Measurements:
The ranges for pH, dissolved oxygen and temperature were 7.14 to 7.93, 6.05 to 8.23 mg/L and 22.8 to 23.7°C, respectively. The acceptable (or recommended) range for pH value is 6.0 to 8.5, dissolved oxygen is at least 5.8 mg/L throughout the test, and the temperature is 21 to 25 °C.

Toxic signs:
During the 14-day exposure period, the fish treated with the test item showed no visible toxic signs and there were no deaths at the limited concentration of 100 mg/L as WAF (nominal concentration).

Body weights and Body Length:
The result of determination of body weight and body length showed that no significant change was found in the control and the test group.

NOEC
The NOEC was 100 mg/L as WAF (with equivalent mean TOC concentration of 24.03 mg TOC/L, and mean determined concentration of neodecanoic acid as 42.2mg/L).

Results with reference substance (positive control):

Not applicable

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

The NOEC was 100 mg/L as WAF (with equivalent mean TOC concentration of 24.03 mg TOC/L, and mean determined concentration of neodecanoic acid as 42.2mg/L).

Executive summary:

E0286P/040A fish, prolonged toxicity test: A 14-day study with zebra fish (Dania rerio) was conducted.

Based on the results of the preliminary test, a definitive test was conducted using a limit test concentration of 100 mg/L, as Water Accommodated Fraction (WAF) (nominal concentration). A concurrent water control group was performed in parallel. The definitive test was performed with a semi-static water renewal system and the water used was reconstituted water (ISO 6341-1982). Dissolved oxygen and pH values were determined at 0-day, 7-day, and 13-day for the fresh and expired solutions during the 14-day exposure period.

During the 14-day exposure period, no toxic signs and deaths were observed for the exposed fish either in the control or the test group.

The concentration of total organic carbon (TOC) was determined in samples of test media. Samples were taken from each test vessel and analyzed in the fresh media at 0-day, 7 -day and 13-day, and in the expired media at 1-day, 8-day and 14-day. The results showed that the mean determined concentration was calculated to be equivalent to 24.03 mg TOC/L in the test media.

The concentration of neodecanoic acid in the test media was monitored by a reverse-phase high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) method, operating under multiple reaction monitoring (MRM) conditions using an external standard. The results showed that the mean concentration of neodecanoic acid was measured as 42.2 mg/L. The result of the 14 days prolonged toxicity test showed the NOEC of the test item E0286P/040A to zebra fish was 100 mg/L as WAF (with an equivalent mean TOC concentration of24.03 mg/L, and a mean determined concentration of neodecanoic acid of 42.2 mg/L).