(2-cyano-1-methylethyl)dodecylethylsulphonium tetrafluoroborate(1-)

Short-term toxicity to fish

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

6 Mar - 28 Apr 2017

Reliability:

4 (not assignable)

Rationale for reliability incl. deficiencies:

other: main test not completed

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

Deviations:

no

GLP compliance:

yes

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Appearance: off-white waxy solid
- Source and lot/batch No.of test material: 629582
- Expiration date of the lot/batch: 9 Dec 2017
- Purity: 98.3%
- Purity test date: 14 Jun 2016

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability under test conditions: Substance is hydrolytically active

Analytical monitoring:

yes

Details on sampling:

- Concentrations: 2.0 mL
- Sampling method: During the test single 2 mL samples were taken from the center of the test vessels. Samples were taken at the start of the test, after 24 hours, and after 96 hours.
- Sample storage conditions before analysis: Samples were transferred to the analytical laboratory at the Test Facility and analysed on the day of sampling.

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION
- Method: All glassware used was silanized to minimise adsorption. Preparation of test solutions started with a loading rate of 100 mg/L applying a two-day period of magnetic stirring to ensure maximum dissolution of the test item in medium. This resulted in a hazy mixture. The aqueous Saturated Solution (SS) was collected by means of filtration through a 0.45 μm membrane filter (RC55, Whatman) and used as the highest test concentration. Lower test concentrations were prepared by subsequent dilutions of the SS in test medium.
- Controls: no
- Evidence of undissolved material: All test solutions were clear and colorless at the end of the preparation.

Test organisms (species):

Danio rerio (previous name: Brachydanio rerio)

Details on test organisms:

TEST ORGANISM
- Common name: Zebra-fish
- Strain: Not reported
- Source: Zodiac, proefacc, "De Haar Vissen", Wageningen University and Research Centre, The Netherlands.
- Age at study initiation (mean and range, SD): Not reported
- Length at study initiation: 2.0 ± 0.2 cm
- Weight at study initiation: 0.06 ± 0.03 g
- Feeding during test: No, fish were not fed 24 hours before the test started or during.

ACCLIMATION
- Acclimation period: At least 12 days after delivery
- Acclimation conditions: Same as test
- Type and amount of food: Pelleted fish food
- Feeding frequency: Daily
- Health during acclimation: Mortality during the seven days prior to the start of the test was less than 5%.

Test type:

static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

96 h

Hardness:

180 mg CaCO3

Test temperature:

21.0 - 21.5 °C

pH:

7.2 - 8.1

Dissolved oxygen:

8.1 - 9.0mg/L

Nominal and measured concentrations:

Nominal: 1.0, 10, 100% saturated solution
Measured: 0.0058, 0.014, and 0.092 μg/L (at start of test, extrapolated from calibration curve)

Details on test conditions:

TEST SYSTEM
- Test vessel: 0.9 litres, all-glass, silanized
- Type: open
- Fill volume: 0.5 litres of test solution
- Aeration: no
- No. of organisms per vessel: 3
- No. of vessels per concentration (replicates): 1
- No. of vessels per control (replicates): none
- Biomass loading rate: 0.36 g fish/L

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Tap water purified by a Milli-Q water purification system (Millipore, Bedford, MA, USA)
- Adjusted ISO medium, formulated using RO-water (tap-water purified by reverse osmosis; GEON Waterbehandeling, Berkel-Enschot, The Netherlands) with the following composition:
CaCl2.2H2O 211.5 mg/L
MgSO4.7H2O 88.8 mg/L
NaHCO3 46.7 mg/L
KCl 4.2 mg/L

OTHER TEST CONDITIONS
- Adjustment of pH: no
- Photoperiod: 16 hours light; 8 hours dark

EFFECT PARAMETERS MEASURED: Mortality and/or severely distressed fish at 3.5, 24, 48, 72, and 96 hours.

Reference substance (positive control):

yes

Remarks:

Pentachlorophenol (PCP)

Key result

Duration:

96 h

Dose descriptor:

LC50

Remarks on result:

not measured/tested

Remarks:

Information became available showing that the test item is subject to rapid hydrolyses

Details on results:

No mortality or clinical effects were observed at any of the test concentrations during the test period. However, the 96h-LC50 for Danio rerio exposed to MTDID 15670 was not determined. The project was stopped in consultation with the sponsor after performance of a range-finding test. Information became available showing that the test item is subject to rapid hydrolysis. The sponsor decided to perform additional testing on the hydrolysis products instead.

Results with reference substance (positive control):

- Results with reference substance valid? yes
- Mortality: yes
- LC50: 0.15 mg/L
- Other: The sensitivity of zebra-fish originating from the present batch for PCP falls within the expected range of sensitivities generally observed for a similar species (carp) during the past years. Reference test was conducted approximately two months after the main test.

Validity criteria fulfilled:

not applicable

Conclusions:

The 96-hour LC50 for Danio rerio exposed to MTDID 15670 according to OECD 203 was not determined. The project was stopped in consultation with the sponsor after performance of a range-finding test. Information became available showing that the test item is subject to rapid hydrolysis.

Executive summary:

The 96-hour LC50 for Danio rerio exposed to MTDID 15670 according to OECD 203 was not determined. No mortality was observed. The project was stopped in consultation with the sponsor after performance of the range-finding tests. Information became available showing that the test item is subject to rapid hydrolysis. Because the test was not completed, the reliability of the results could not be assigned.

Reference 2

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

weight of evidence

Study period:

26 Feb - 31 Mar 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

Deviations:

no

GLP compliance:

yes

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- State of substance: clear colourless liquid
- Source and lot/batch No.of test material: Sigma-Aldrich Chemie GmbH, Steinheim, Germany, batch: STBD0697V
- Purity: 99.8%, mixture of cis and trans

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: at room temperature

Analytical monitoring:

yes

Details on sampling:

- Concentrations: control (test medium without test item) and 100 mg/L
- Sampling method: Duplicate samples (6.0 mL) for analysis were taken from both test groups at the start of the test and at 96 hours. In addition, a quality control sample of 3.0 mL was taken from the limit concentration at the start and the end of the test period.

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION
- Method: Preparation of test solutions started with the highest concentration of 100 mg/L applying 10 minutes of magnetic stirring to accelerate dissolution of the test item in medium. Lower test concentrations were prepared by subsequent dilutions of the highest concentration in test medium.
- Controls: Test medium without test item or other additives
- Evidence of undissolved material: All test solutions were clear and colorless at the end of the preparation procedure.

Test organisms (species):

Danio rerio (previous name: Brachydanio rerio)

Details on test organisms:

TEST ORGANISM
- Common name: Zebra fish
- Source: Zodiac, proefacc, “De Haar Vissen”, Wageningen University and Research Centre, the Netherlands
- Length at study initiation (mean): Range-finding test: 2.9 ± 0.1 cm; Limit test: 2.9 ± 0.2 cm
- Weight at study initiation (mean): Range-finding test: 0.27 ± 0.07 g; Limit test: 0.22 ± 0.06 g

ACCLIMATION
- Acclimation period: at least 12 days after delivery
- Acclimation conditions: Adjusted ISO medium, formulated using RO-water (tapwater purified by reverse osmosis; GEON Waterbehandeling, Berkel-Enschot, The Netherlands) with the following composition:
CaCl2.2H2O 211.5 mg/L
MgSO4.7H2O 88.8 mg/L
NaHCO3 46.7 mg/L
KCl 4.2 mg/L
- Type and amount of food during acclimation: pelleted fish food (Cyprico Crumble Excellent (300-500 um), Coppens International bv, Helmond, The Netherlands)
- Feeding frequency during acclimation: daily until 24 hours prior to the start of the test
- Health during acclimation (any mortality observed): less than 5% mortality in the seven days prior to the test

FEEDING DURING TEST
- No feeding from 24 hours prior to the test and during the total test period.

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

96 h

Hardness:

180 mg CaCO3/L

Test temperature:

22 - 23 °C

pH:

7.5 - 7.9

Dissolved oxygen:

7.4 - 9.4 mg/L

Nominal and measured concentrations:

Nominal: 100 mg/L
Measured: 83 mg/L

Details on test conditions:

TEST SYSTEM
- Test vessel: 6.5 L glass vessel
- Fill volume: 5 L
- Aeration: no
- No. of organisms per vessel: 7
- No. of vessels per concentration (replicates): 1
- No. of vessels per control (replicates): 1
- Biomass loading rate: 0.31 g fish/L

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: adjusted ISO medium with a hardness of 180 mg CaCO3 per litre and a pH of 7.7 ± 0.3, prepared using reverse-osmosis purified water (GEON Waterbehandeling, Berkel-Enschot, The Netherlands) with the following composition:
CaCl2.2H2O 211.5 mg/L
MgSO4.7H2O 88.8 mg/L
NaHCO3 46.7 mg/L
KCl 4.2 mg/L
- Intervals of water quality measurement: Daily in all vessels with surviving fish, beginning at the start of the test (day 0)

OTHER TEST CONDITIONS
- Adjustment of pH: no
- Photoperiod: 16 hours light; 8 hours dark

EFFECT PARAMETERS MEASURED:
Mortality and/or severely distressed fish at 4, 24, 48, 72, and 96 hours.

TEST CONCENTRATIONS
- Range finding study: 0.1, 1.0, 10, and 100 mg/L
- Test concentrations: 100 mg/L

Reference substance (positive control):

yes

Remarks:

pentachlorophenol (PCP)

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 83 mg/L

Nominal / measured:

meas. (geom. mean)

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Remarks on result:

other: No mortality at highest concentration tested

Details on results:

- Behavioural abnormalities: none
- Mortality of control: None
- Other adverse effects control: None
- Other: In a range-finding study, after 72 hours of exposure, hemorrhages, abnormal swimming behaviour (i.e. close to the surface) and a swollen abdomen was observed in one fish which eventually died within the following 8 hours.

Results with reference substance (positive control):

- Results with reference substance valid? yes
- Mortality: yes
- LC50: 0.15 mg/L
- Other: The sensitivity of zebra-fish originating from the present batch for PCP falls within the expected range of sensitivities generally observed for a similar species (carp) during the past years. Reference test was conducted within one year.

Validity criteria fulfilled:

yes

Remarks:

No control mortality, DO > 60% of saturation, results are based on average exposure concentration calculated at the limit concentration

Conclusions:

The 96-hour LC50 of crotononitrile, a hydrolysis product of MTDID 15670, to Danio rerio was > 83 mg/L (OECD 203).

Executive summary:

The 96-hour LC50 of crotononitrile, a hydrolysis product of MTDID 15670, to zebra-fish (Brachydanio rerio) was examined in a static, limit test conducted according to OECD TG 203. Test solutions were prepared as the control (0 mg/L) and at 100 mg/L. No mortality or other clinical effects were observed at the 100 mg/L loading rate or in controls. The study was well-documented, followed an international standard method, and was GLP compliant; therefore, the test is considered reliable without restriction.

Reference 3

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

weight of evidence

Study period:

1990

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study without detailed documentation

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

GLP compliance:

yes

Specific details on test material used for the study:

50% solution of tetrafluoroboric acid

Analytical monitoring:

yes

Remarks:

Analytical monitoring was reported, but no details were provided.

Test organisms (species):

Danio rerio (previous name: Brachydanio rerio)

Details on test organisms:

Test organism reported using previous name: Brachydanio rerio

Test type:

static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

96 h

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

1 300 mg/L

Nominal / measured:

meas. (not specified)

Conc. based on:

act. ingr.

Basis for effect:

mortality (fish)

Remarks on result:

other:

Remarks:

Result reported as LC50 = 2.6 g/L for the test substance, 50% HBF4. It was not reported if the result was based on active ingredient or test material. Conservatively, the result was assumed to be for the test material, therefore the LC50 = 1300 mg/L for HBF4.

Validity criteria fulfilled:

not specified

Conclusions:

The 96-hour LC50 of tetrafluoroboric acid is 1300 mg/L, as determined according to the OECD TG 203 method. Tetrafluoroboric acid is a hydrolysis product of MTDID 15670.

Executive summary:

The toxicity of tetrafluoroboric acid, a hydrolysis product of MTDID 15670, to Danio rerio was examined in a static test conducted according to OECD TG 203. The result was documented in an IUCLID report, and was reported to have been conducted with analytical monitoring and to have been GLP compliant, however details of the study were not published. The test material was identified as 50% HBF4, but it was not reported if the result was for the active ingredient or the test material. Conservatively, it was assumed that the result was for the test material, and thus the 96-hr LC50 is 1300 mg/L. Although details of the study were not available, the result is considered reliable with restrictions, since the study was conducted according to OECD TG 203 and was GLP compliant.

Reference 4

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

weight of evidence

Study period:

02-March-2018 to 16-March-2018

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

Deviations:

no

GLP compliance:

yes

Specific details on test material used for the study:

Dodecyl methyl sulfide is used within this study as a surrogate for dodecyl ethyl sulfide, which is a hydrolysis product of MTDID 15670. Dodecyl ethyl sulfide is not commercially available.
SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: Sigma-Aldrich, Batch Number MKBW6054V
- Physical state: colorless, liquid
- Quality Release Date: 12JAN20
- Purity: 97.8%
- Storage condition of test material: room temperature

Analytical monitoring:

yes

Details on sampling:

- Concentrations: negative control and saturated solution (limit test)
- Volume: Control: 3 mL for the regular samples and 1.5 mL for quality control (QC) samples
- Sampling method: Duplicate samples for analysis, and duplicate reserve samples, were taken from the approximate center of the test vessels. Two extra samples were taken from the limit concentration for analytical QC, and two reserve QC samples were also taken. Samples were taken at test initiation (T = 0 h) and test completion (T= 96 h).
- Sample storage conditions before analysis: Samples were transferred to the analytical laboratory at the test facility on the day of sampling for extraction then stored in a freezer (≤ -15°C) until analyses.

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION
- Method: The batch of dodecyl methyl sulfide tested was a colorless liquid which was not completely soluble in test medium at the initially prepared loading rate. Preparation of test solutions started with a loading rate of 100 mg/L (501.0 mg/ in 5 liters) applying a two-day period of gentle magnetic stirring to ensure maximum dissolution of the test item in medium. The obtained mixture was allowed to settle for an overnight period. Thereafter, the aqueous Saturated Solution (SS) was collected by means of siphoning and used as the highest test concentration.
- Controls: Blank only
- Evidence of undissolved material (e.g. precipitate, surface film, etc.): Test solutions were clear and colorless at the end of the preparation procedure.

Test organisms (species):

Danio rerio (previous name: Brachydanio rerio)

Details on test organisms:

TEST ORGANISM
- Common name: Zebra-fish
- Source: Zodiac, proeffac, De Haar Vissen, Wageningen University and Research Centre, The Netherlands
- Length at study initiation: 2.9 ± 0.2 cm
- Weight at study initiation: 0.22 ± 0.06 g
- Feeding during test: no

ACCLIMATION
- Acclimation period: At least 12 days after delivery
- Acclimation conditions: Adjusted ISO medium, formulated using RO-water (tapwater purified by reverse osmosis; GEON Waterbehandeling, Berkel-Enschot, The Netherlands) with the following composition:
CaCl2.2H2O 211.5 mg/L
MgSO4.7H2O 88.8 mg/L
NaHCO3 46.7 mg/L
KCl 4.2 mg/L
- Type and amount of food during acclimation: pelleted fish food (Essence (300-500 um), Coppens International bv, Helmond, The Netherlands)
- Feeding frequency during acclimation: daily until 24 hours prior to the start of the test
- Health during acclimation (any mortality observed): less than 5% mortality in the seven days prior to the test

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

96 h

Hardness:

180 mg CaCO3/L

Test temperature:

22.1 °C to 23.2 °C

pH:

7.5 to 7.9

Dissolved oxygen:

7.0 mg/L to 9.3 mg/L

Nominal and measured concentrations:

Nominal: Blank and 100 mg/L loading level
Measured: Below the Limit of Detection (LOD, i.e. < 0.0102 mg/L) for all samples

Details on test conditions:

TEST SYSTEM
- Test vessel: 6.5 L glass flasks
- Fill volume: 4.5 L
- Aeration: no
- No. of organisms per vessel: 7
- No. of vessels per concentration: one
- No. of vessels per control: one
- Biomass loading rate: 0.34 g fish/L
TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Adjusted ISO medium, formulated using RO-water (tap-water purified by
reverse osmosis; GEON Waterbehandeling, Berkel-Enschot, The Netherlands)
OTHER TEST CONDITIONS
- Adjustment of pH: no
- Photoperiod: 16 hours light; 8 hours dark
EFFECT PARAMETERS MEASURED: mortality and other effects at 3.75, 24, 48, 72, and 96 hours
following the start of exposure. In addition, every afternoon from day 0 to observe for any dead or
severly distressed fish.
TEST CONCENTRATIONS
- Test concentrations: 100 mg/L loading level
RANGE-FINDING STUDY
- Test concentrations:0 mg/L (blank), 100 mg/L (nominal loading rate)
- Results used to determine the conditions for the definitive study: yes

Reference substance (positive control):

yes

Remarks:

Pentachlorophenol (PCP)

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Remarks on result:

other:

Remarks:

No mortality or clinical effects at only concentration tested.

Details on results:

- Behavioural abnormalities: no
- Mortality of control: no
- Other adverse effects control: no
- Abnormal responses: no
- Effect concentrations exceeding solubility of substance in test medium: yes

Results with reference substance (positive control):

- Results with reference substance valid? yes
- Mortality: yes
- LC50: 0.15 mg/L (95% confidence interval between 0.10 and 0.22 mg/L)
- Other: Sensitivity trend data for this species are still being collected. The sensitivity of zebra-fish originating from the present batch for PCP falls within the expected range of sensitivities generally observed for a similar species (carp) during the past years. The reference substance test was conducted ten months before the testing of dodecyl methyl sulfide.

Validity criteria fulfilled:

yes

Remarks:

No control mortality, DOC > 60% of saturation

Conclusions:

The 96-hour LC50 of dodecyl methyl sulfide to zebra-fish (Danio rerio) was found to be > 100 mg/L (nominal) in a limit test per OECD 203. No toxicity was observed. The loading rate exceeded the maximum soluble concentration for dodecyl methyl sulfide in test medium.

Executive summary:

The 96-hour LC50 of dodecyl methyl sulfide to zebra-fish (Brachydanio rerio) was examined in a static, limit test conducted according to OECD TG 203. Dodecyl methyl sulfide is a surrogate for dodecyl ethyl sulfide (not commercially available), an expected hydrolysis product of MTDID 15670. Test solutions were prepared as the control (0 mg/L) and as a water soluble fraction at a loading rate of 100 mg/L. No mortality or other clinical effects were observed at the 100 mg/L loading rate or in the control. The measured concentration of dodecyl methyl sulfide was below the Limit of Detection (< 0.0102 m/gL) for all samples. The study was well-documented, followed an international standard method, and was GLP compliant. The study is considered reliable with restrictions. The results from this study are considered suitable for Risk Assessment, Classification and Labeling, and PBT Analysis.

Description of key information

MTDID 15670 hydrolyzes rapidly (T1/2 < 12 hrs) in water. Results from short-term toxicity tests (OECD TG 203) with the hydrolysis products of MTDID 15670 (or a surrogate chemical) all indicate that with zebra-fish (Danio rerio, formerly Brachydanio rerio) the 96-hour LC50 is > 100 mg/L.

Additional information

A preliminary short-term toxicity to fish study (OECD 203) with MTDID 15670 for Danio rerio was initiated, but stopped after consultation with the sponsor, after encountering phase separation (precipitation) during the range-finding test. No mortality was observed in the range-finding test. Subsequently, information became available showing that MTDID 15670 is subject to rapid hydrolysis. Because the test was not completed, the reliability of the results could not be assigned. Analysis after hydrolysis revealed three products; two chemicals with moderate water solubility, crotononitrile (CAS# 4786-20-3) and tetrafluoroborate anion (tetrafluoroboric acid, CAS# 16872-11-0), along with the poorly soluble chemical, dodecyl ethyl sulfide (No CAS#). Short-term toxicity testing results for these hydrolysis products follow.

The 96-hour LC50 of crotononitrile, to zebra-fish (Danio rerio) was examined in a static, limit test conducted according to OECD TG 203. Test solutions were prepared as the control (0 mg/L) and at 100 mg/L. No mortality or other clinical effects were observed at the 100 mg/L loading rate or in controls. The measured concentration at the highest loading rate was 83 mg/L. The study was well-documented, followed an international standard method, and was GLP compliant; therefore, the test is considered reliable without restriction.

The 96-hour LC50 of dodecyl methyl sulfide (CAS# 3698-89-3) to zebra-fish (Danio rerio) was examined in a static, limit test conducted according to OECD TG 203. Dodecyl methyl sulfide is a surrogate for dodecyl ethyl sulfide (not commercially available). Test solutions were prepared as the control (0 mg/L) and as a water soluble fraction at a loading rate of 100 mg/L. No mortality or other clinical effects were observed at the 100 mg/L loading rate or in the control. The measured concentration of dodecyl methyl sulfide was below the Limit of Detection (< 0.0102 m/gL) for all samples. The study was well-documented, followed an international standard method, and was GLP compliant. The study is considered reliable with restrictions. The results from this study are considered suitable for Risk Assessment, Classification and Labeling, and PBT Analysis.

The toxicity of tetrafluoroboric acid, to Danio rerio was examined in a static test conducted according to OECD TG 203. The result was documented in an IUCLID report, and was reported to have been conducted with analytical monitoring and to have been GLP compliant, however details of the study were not published. The test material was identified as 50% HBF4, but it was not reported if the result was for the active ingredient or the test material. Conservatively, it was assumed that the result was for the test material, and thus the 96-hr LC50 is 1300 mg/L. Although details of the study were not available, the result is considered reliable with restrictions, since the study was conducted according to OECD TG 203 and was GLP compliant.