Reaction mass of nonane-1,3-diyl diacetate and tetrahydro-3-pentyl-2H-pyran-4-yl acetate

Short-term toxicity to aquatic invertebrates

Administrative data

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

January 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

no

GLP compliance:

no

Test material

Test material information

Constituent 1

Reference substance name:

Tetrahydro-3-pentyl-2H-pyran-4-yl acetate

EC Number:

242-640-5

EC Name:

Tetrahydro-3-pentyl-2H-pyran-4-yl acetate

Cas Number:

18871-14-2

Molecular formula:

C12H22O3

IUPAC Name:

3-O-acetyl-1,5-anhydro-2,4-dideoxy-2-pentylpentitol

Constituent 2

Reference substance name:

Nonane-1,3-diyl diacetate

EC Number:

264-060-1

EC Name:

Nonane-1,3-diyl diacetate

Cas Number:

63270-14-4

Molecular formula:

C13H24O4

IUPAC Name:

nonane-1,3-diyl diacetate

impurity 1

Reference substance name:

1-(tetrahydrofuran-3-yl)hexyl acetate

Molecular formula:

C12H22O3

IUPAC Name:

1-(tetrahydrofuran-3-yl)hexyl acetate

impurity 2

Reference substance name:

rel-(3R,4R)-3-pentyltetrahydro-2H-pyran-4-ol

Cas Number:

24646-98-8

Molecular formula:

C10H20O2

IUPAC Name:

rel-(3R,4R)-3-pentyltetrahydro-2H-pyran-4-ol

impurity 3

Reference substance name:

3-hydroxynonyl acetate

Cas Number:

902270-36-4

Molecular formula:

C11H22O3

IUPAC Name:

3-hydroxynonyl acetate

Test material form:

liquid

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: PE00120812
- Expiration date of the lot/batch: 09 Jul 2017
- Purity test date: 78.4% (two main peaks)

Sampling and analysis

Analytical monitoring:

yes

Details on sampling:

0h, 24h before medium exchange, 24h after medium exchange and at 48 h

Test solutions

Vehicle:

no

Details on test solutions:

The test was conducted by preparing a saturated solution, which was diluted to achieve a final concentration of 33%, 16.5%, 8.25%, 4.125% and 2.063 % of a saturated solution (effective concentrations 91.2, 48.0, 23.9, 11.3 and 5.7 mg/L based on mean measured concentrations). A control group was also included. The test concentrations were based on a limited range-finder test. The minimal dilution of the saturated solution was chosen to achieve a maximal test concentration of around 100 mg/L in the main test.

Test organisms

Test organisms (species):

Daphnia magna

Details on test organisms:

The test organism Daphnia magna, in the form of ephippia, was obtained from MicroBio Test Inc, Mariakerke (Gent), Belgium. Hatching was initiated 3 days prior to the start of the toxicity test.

Study design

Test type:

semi-static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

48 h

Test conditions

Test temperature:

The laboratory temperature was set within the range 21 to 24°C and maintained within ± 2°C for the duration of the test.

pH:

At the start of the test, the pH and the oxygen saturation of freshly prepared test water and the saturated solution were determined. The pH and the oxygen saturation in one replicate of the maximal test concentration and the control were also determined at the start, the 24 h renewal time and at the end of the test. See table 3 in attached report for more information.

Dissolved oxygen:

At the start of the test, the pH and the oxygen saturation of freshly prepared test water and the saturated solution were determined. The pH and the oxygen saturation in one replicate of the maximal test concentration and the control were also determined at the start, the 24 h renewal time and at the end of the test.

Nominal and measured concentrations:

Range-finder: Nominal concentrations of 1, 5, and 25 mg/L (solvent spike set up) were tested and time-weighted mean measured concentrations of 0.94, 4.95 and 16.56 mg/L were achieved in this test.
Main Test: Nominal concentrations of 2.063, 4.125, 8.25, 16.5 and 33 % of saturated solution; equivalent to time-weighted mean measured concetrations of 5.65, 11.25, 23.93, 48.00 and 91.19 mg/L

Details on test conditions:

Sealed with minimum headspace to minimize any potential loss due to volatility

Reference substance (positive control):

yes

Remarks:

Potassium Dichromate

Results and discussion

Effect concentrations

Effect concentrations 1

Key result

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

55 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

mobility

Effect concentrations 2

Duration:

48 h

Dose descriptor:

LOEC

Effect conc.:

24 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

mobility

Effect concentrations 3

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

11.3 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

mobility

Details on results:

Analysis of the test samples at the start of the exposure intervals (0 and 24 hours) showed measured concentrations to range from 5.7 to 92.5 mg/L and at the end of the exposure intervals (24 and 48 hours) to range from 5.5 to 96.8 mg/L.

The measured concentrations were calculated by summing up the area of the two peaks of the main components of Jasmonyl. Example chromatograms of standard solutions (Figure 1 and 2) and of test samples (Figures 3 to 6) are provided in the full study report. The peak at 11.5 contains the 3-pentyltetrahydro-2H-pyran-4-yl acetate isomers while the peak at 12.5 corresponds to nonane-1,3-diyl diacetate. The ratio of the first to the second main peak in the test sample is at 2.8. Due to the lower water solubility of the second peak, the main peak is further enriched in the saturated solution and in all test samples (ratio of first to second peak 7.85; see Figures 3 - 6 in the full study report).

All results have been based on time weighted mean measured concentrations.

Results with reference substance (positive control):

The EC50 was determined to be 0.9 mg/L after 24 h and at 0.63 mg/L after 48 h. The result of the internal ring trial cited in OECD TG 202 for EC50 is 0.6 mg/L – 2.1 mg/L after 24 h. Thus, these results were within the expected range.

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

After 48 hours, the concentration at which no significant (≤10%) dose related immobility occurred was 11.3 mg/L. The NOEC was thus considered to be 11.3 mg/L. After 48 hours 100% immobility was recorded at the highest test concentration of 91.2 mg/L.
In terms of time-weighted mean measured concentrations, the 48-hour EC50 value was determined to be 55.0 mg/L and the LOEC to be 24.0 mg/L.
The validity criteria for control immobility (≤10%) and dissolved oxygen (≥3 mg/L) were both satisfied. The test is therefore considered valid.