1,3-Propanediol, 2,2-bis(hydroxymethyl)-, allyl ether

Bioaccumulation: aquatic / sediment

Link to relevant study record(s)

Reference

Endpoint:

bioaccumulation in aquatic species: fish

Type of information:

experimental study

Adequacy of study:

key study

Study period:

17/02/2022 to 10/05/2022

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

OECD 305-I

Qualifier:

according to guideline

Guideline:

OECD Guideline 305 (Bioaccumulation in Fish: Aqueous and Dietary Exposure) -I: Aqueous Exposure Bioconcentration Fish Test

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL:
-Source: Perstorp AB
-Batch no. 210509236
-Expiry date 21 November 2022
STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL:
-Ambient. Protect from Direct Sunlight. Cover with nitrogen after removing any material from container
-Liquid

Radiolabelling:

no

Remarks:

Radiolabeling was not suitable for the study design OECD 305-I.

Details on sampling:

- Sampling intervals/frequency for test organisms:
Fish samples were taken in four replicates starting from the first day of the uptake phase and continued on 1d, 2d, 4d, 7d, and 14d during the uptake phase. The depuration phase sampling was performed from 18d, and continued on 19d, 20d and 21d.
- Sampling intervals/frequency for test medium samples:
Sampling of 3 main constituents of Allyl Pentaerythritol (APE) was taken at different occasions. Water samples were taken in two replicates starting from -3d, -2d, -1d, 0d, 1d, 2d, 4d, 7d, and 14d during the uptake phase. The depuration phase sampling was performed from 18d, and continued on 19d, 20d and 21d.
- Sample storage conditions before analysis: Sample was kept in the freezer prior analysis.
Samples were analyzed on the same day.
- Details on sampling and analysis of test organisms and test media samples (e.g. sample preparation, analytical methods):
In each analytical batch of water and fish samples, a fresh set of derivatised calibration solutions was prepared with BSTFA with 1% TMCS concurrently with the derivatisation of sample extracts.
Concentrations of the 3 main components of APE were determined using the validated method in the following fish samples from the test group. Whole fish were homogenised prior to analysis. further detail on the analytical method has been described on the "Details on the analytical method" section.

Vehicle:

yes

Remarks:

Dosing solution was prepared by dissolving APE in dimethylformamide (DMF) and this solution was diluted with water to provide the test water

Details on preparation of test solutions, spiked fish food or sediment:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
- Method: A HPLC pump was used to continuously deliver dosing solution into a glass mixing vessel, where it was mixed with dilution water. Test solutions were aerated at all times and were delivered to each tank from Day -5.
- Controls: A HPLC pump was used to continuously deliver DMF for the control group. Control solutions were aerated at all times and were delivered to each tank from Day -5.
- Chemical name of vehicle (organic solvent, emulsifier or dispersant): dimethylformamide (DMF)
- Concentration of vehicle in test medium (stock solution and final test solution(s) at different concentrations and in control(s)): In a 10,000 µg/mL stock solution of APE, 5ml of DMF was administered.

Test organisms (species):

Oncorhynchus mykiss (previous name: Salmo gairdneri)

Details on test organisms:

TEST ORGANISM
- Common name: Rainbow trout
- Source: Northern Trout Ltd. UK.
- Length at study initiation (length definition, mean, range and SD): 48mm
- Weight at study initiation (mean and range, SD): 0.86± 0.1g
- Weight at termination (mean and range, SD): 1,92 ± 0.25g
- Lipid content at test initiation (mean and range, SD): 0.89% w/w
- Health status: Fish were not treated for any disease during the acclimatisation period or during the testing (uptake/depuration) period. No fish died during the study period.
- Description of housing/holding area: Glass aquaria tanks (ca. 140 L volume) containing ca. 120L of water were used to house the fish during the uptake and depuration phases.
-Temperature: control tank 13.5-15.5 °C, test tank 13.5-14.5 °C
-Aeration: Continuous aeration
-Light: 610-856 lux
- Feeding during test
- Food type: trout pellets (BioMar Inicio Plus)
- Amount: 1.9-2% of body weight per day
- Frequency: Once per day

ACCLIMATION
- Acclimation period: 15days prior starting of the test
- Acclimation conditions (same as test or not): same as the test condition
-Temperature: The temperature during acclimatisation was measured to be 13.5-14 °C .
-Aeration: Continuous aeration
- Type and amount of food: 1.75% of body weight per day
- Feeding frequency: Once per day
- Health during acclimation (any mortality observed):No fish died during acclimatisation and the acclimatised fish were therefore accepted for use in the test and control groups.

Route of exposure:

aqueous

Justification for method:

aqueous exposure method used for following reason: The route of exposure is through the aquatic environment.

Test type:

flow-through

Water / sediment media type:

natural water

Remarks:

Dechlorinated mains water

Total exposure / uptake duration:

ca. 14 d

Total depuration duration:

ca. 4 d

Hardness:

See Table no. Table 3

Test temperature:

13.5-14 °C

pH:

See Table no. 4

Dissolved oxygen:

See Table no. Table 5

TOC:

See Table no. Table 6

Salinity:

Since, the study was performed in the natural freshwater with a freshwater species, measurement of the salinity was not required.

Details on test conditions:

TEST SYSTEM
- Test vessel, Material, size, headspace, fill volume: Glass aquaria tanks (ca. 140 L volume) containing ca. 120 L of water were used to house the fish during the uptake and depuration phases.
- Type (delete if not applicable): open system
- Aeration: all the time aerated during the test period
- Renewal rate of test solution (frequency/flow rate):The flow rate of the test and control water was equivalent to approximately 5 volume changes per 24 hours. Measured flows were within 1% of target of 600 L/day during uptake and depuration.
- No. of organisms per vessel: 8o fishes in both control and treatment vessel
- No. of vessels per concentration (replicates): 1 vessel
- No. of vessels per control / vehicle control (replicates): 1 vessel per control

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Dechlorinated mains water
- Particulate matter: Please see table 3
- Alkalinity: Please see table 3
- Holding medium different from test medium: No
- Intervals of water quality measurement: 7days of interval during the uptake phase and the sample was checked on the 4th day of depuration time (0d, 7d, 14d, 21d=4th day of depuration)
- Intervals of test medium replacement: continuous renewal

OTHER TEST CONDITIONS
- Adjustment of pH: pH was within ±0.5 pH units of value during the test period, please see table 4
- Photoperiod: 16h:8h, light: dark photoperiod was maintained everyday (24h) with 20 minutes of dusk and dawn.
- Light intensity: Measured light intensity at the water surface was in the range 610-856 lux

Nominal and measured concentrations:

single target nominal concentration of 0.5 mg/L (= 0.5 µg/mL)

Reference substance (positive control):

not required

Remarks:

The lab has previous experience with the test and there was no change in the experimental condition.

Lipid content:

ca. 4.96 other: % w/w

Time point:

other: end of depuration phase

Remarks on result:

other: 4d of depuration

Lipid content:

ca. 3.17 other: % w/w

Time point:

other: End of the uptake phase

Remarks on result:

other: 14d of uptake phase

Lipid content:

ca. 0.89 other: % w/w

Time point:

start of exposure

Remarks on result:

other: 0 day

Key result

Conc. / dose:

ca. 100 other: µg/mL

Temp.:

ca. 13.5 - 14.5 °C

pH:

8.31

Type:

BCF

Value:

< 26 L/kg

Basis:

normalised lipid fraction

Calculation basis:

steady state

Remarks:

The data was not suitable for kinetic analysis for Pentaerythritol diallyl ether because fish concentrations were below the LOQ of the analytical method in all samples analysed.

Remarks on result:

other: Pentaerythritol diallyl ether

Key result

Conc. / dose:

ca. 100 other: µg/mL

Temp.:

ca. 13.5 - 14.5 °C

pH:

8.31

Type:

BCF

Value:

< 34 L/kg

Basis:

normalised lipid fraction

Calculation basis:

steady state

Remarks:

The data was not suitable for kinetic analysis for Pentaerythritol triallyl ether because fish concentrations were below the LOQ of the analytical method in all samples analysed.

Remarks on result:

other: Pentaerythritol triallyl ether

Key result

Conc. / dose:

ca. 100 other: µg/mL

Temp.:

ca. 13.5 - 14.5 °C

pH:

8.31

Type:

BCF

Value:

ca. 120 L/kg

Basis:

normalised lipid fraction

Calculation basis:

kinetic, corrected for growth

Remarks on result:

other: Pentaerythritol tetraallyl ether

Key result

Conc. / dose:

ca. 100 other: µg/mL

Temp.:

ca. 13.5 - 14.5 °C

pH:

8.31

Type:

BCF

Value:

ca. 117 L/kg

Basis:

other: steady state

Calculation basis:

steady state

Remarks on result:

other: Pentaerythritol tetraallyl ether

Key result

Elimination:

yes

Parameter:

DT90

Depuration time (DT):

2.19 d

Remarks on result:

other: Pentaerythritol tetraallyl ether

Key result

Elimination:

yes

Parameter:

DT50

Depuration time (DT):

0.658 d

Remarks on result:

other: Pentaerythritol tetraallyl ether

Key result

Rate constant:

growth-corrected depuration rate constant (d-1)

Value:

1.05

Remarks on result:

other: Pentaerythritol tetraallyl ether

Details on kinetic parameters:

The data was not suitable for kinetic analysis for components for which fish concentrations were below the LOQ of the analytical method in all samples analysed as a result, the following parameters were possible to measure only for Pentaerythritol tetraallyl ether,
- Uptake rate constant k(s): 150 L kg-1 day-1
- Depuration rate constant k(e): 1.09 day-1
- Computation / data analysis: with 95% confidence interval using Box-Cox transformed fit to fish concentration from bcmfR V 0.4-18’ package,

Results with reference substance (positive control):

Not applicable

Details on results:

No abnormalities were observed in swimming behavior, ventilatory function or appearance in any of the test or control fish during the uptake or depuration phases.

Reported statistics:

For components for which fish concentrations were above the LOQ in samples from the uptake phase, the following parameters were obtained from a non-linear regression model of concentration data in fish using the software package ‘bcmfR V 0.4-18’ for the statistical software environment ‘R V 3.4.4’:
• The uptake rate constant k1 (L kg-1 day-1) and deputation rate constant k2 (day-1).
• The growth corrected depuration rate constant k2G (day-1), calculated as k2 – kG.
• The growth corrected depuration half-life DT50 (day) = Loge(2)/k2G.
• The kinetic bioconcentration factor BCFK (L kg-1) = k1/k2.
• The growth-corrected kinetic bioconcentration factor BCFKG (L kg-1) = k1/k2G
• The lipid-normalised growth-corrected kinetic bioconcentration factor BCFKLG (L kg-1) = (BCFKG) x (LN)
• If steady-state fish concentrations had been reached then the steady state bioconcentration factor (BCFSS) = CF,SS/CW

The following factors, which are not specific to the components of APE, were calculated:     Estimate 95% CI LN lipid normalisation factor 1.577 ---- kG overall fish growth rate constant (day^-1), 0.0327 (0.0281, 0.0374) Pentaerythritol diallyl ether The data for this component was not suitable for kinetic analysis since fish concentrations were below the LOQ of the analytical method in all samples analysed.  The following parameters were calculated:     Estimate 95% CI BCFSS steady state BCF (L kg^-1) <16 ---- BCFSSL lipid-normalised steady state BCF (L kg^-1) <26 ---- Pentaerythritol triallyl ether The data for this component was not suitable for kinetic analysis since fish concentrations were below the LOQ of the analytical method in all samples analysed.  The following parameters were calculated:     Estimate 95% CI BCFSS steady state BCF (L kg^-1) <21 ---- BCFSSL lipid-normalised steady state BCF (L kg^-1) <34 ---- Pentaerythritol tetraallyl ether The Box-Cox transformed fit of fish concentration, with 95% confidence intervals, is shown in Figure 28.  The kinetic parameters derived from the ‘bcmfR V 0.4-18’ package were estimated using this fit.  Concentrations in fish were stable during the uptake phase allowing a steady-state bioconcentration factor (BCF) to be calculated along with a lipid-corrected steady-state BCF (normalised to 5% fish lipid content).  Steady state parameters were estimated using fish and water concentrations on days 2, 7 and 14. The following parameters were calculated.  The 95% confidence limit (95% CI) is also listed when calculated.     Estimate 95% CI BCFSS steady state BCF (L kg^-1) 117 (104, 130) BCFSSL lipid-normalised steady state BCF (L kg^-1) 185 (164, 206) k1 uptake rate constant (L kg^-1 day^-1) 130 (111, 150) k2 deputation rate constant (day^-1) 1.09 (0.96, 1.21) k2G growth corrected depuration rate constant (day^-1) 1.05 (0.93, 1.18) DT50 growth-corrected depuration half-life (day) 0.658 (0.580, 0.736) DT90 growth-corrected time of 90% depuration (day) 2.19 ---- BCFK kinetic BCF (L kg^-1) 120 (111, 129) BCFKG growth-corrected kinetic bioconcentration factor (L kg^-1) 124 (114, 133) BCFKL lipid-normalised kinetic bioconcentration factor (L kg^-1) 189 ---- BCFKLG lipid-normalised growth-corrected kinetic bioconcentration factor (L kg^-1) 195 (181, 210)

Validity criteria fulfilled:

yes

Remarks:

water temperature variation was of less than ± 2 ˚C, dissolved oxygen concentration was above 60 % saturation, test item concentration in water during uptake was within ± 20 % of the mean value, Mortality < 10 % in both test and control fish

Conclusions:

The study was judged to be valid. Estimates of steady state BCF (117 L kg-1) and kinetic BCF (120 L kg-1) were in good agreement.

Executive summary:

Concentrations of pentaerythritol diallyl ether and pentaerythritol triallyl ether in fish were below the LOQ (1.1 mg/kg and 7.9 mg/kg respectively) at days 2, 7 and 14. Therefore, data obtained on those components of APE were unsuitable to calculate the BCFkinetics. steady state and lipid normalized steady state BCF shows that these to constituents are not bioaccumulative in fish tissue. 

Concentrations of pentaerythritol tetraallyl ether in fish rose rapidly after the start of the uptake phase and were above the LOQ (0.97 mg/kg) by Day 2 and by day 14, the equilibrium concentration was reached.

After 1 day of depuration, pentaerythritol diallyl ether and, pentaerythritol triallyl ether were no longer detectable in fish.  Concentrations of pentaerythritol tetraallyl ether were above the LOQ in all 4 fish samples taken on Day 1 of depuration but this component was undetectable or barely detectable in fish from Day 4 of depuration.

BCFsteady state was 117L kg^-1 and the BCFkinetics is 120L kg^-1 which is way below the criteria of fulfilling the bioaccumulative, (B, BCF >2000) and very Bioaccumulative (vB, BCF>5000) property of a substance in the PBT assessment (REACH ANNEX XIII, 1.1.2. and 1.2.2.).

Overall, this substance is neither bioaccumulative (B) nor very Bioaccumulative (vB) in nature.

Description of key information

Indirect exposure of the aquatic compartment is likely.  Based on the log PoW data,  of the main components of 1,3-Propanediol, 2,2-bis(hydroxymethyl)-, allyl ether at 25°C, the bioaccumulation potential of 1,3-Propanediol, 2,2-bis(hydroxymethyl)-, allyl ether was considered uncertain based on log Pow alone. Therefore in accordance with Column 2 of Annex IX of the REACH regulation a fish bioaccumulation study was proposed to assess the bioacculation potential of the substance. 

A Bioconcentration study on the Primary Components of Allyl Pentaerythritol (APE) in Fish: Aqueous Exposure Test OECD 305-I was performed recently where, the BCF of 3 major constituents of APE was calculated. The highest BCF (BCF_kinetics: 120 Lkg^-1 , BCF_{steady state}: 117 Lkg^-1) was obtained from Pentaerythritol tetraallyl ether which is the contributes 9.5% of the total APE. The BCF of the rest two constituents (Pentaerythritol ditraallyl ether and Pentaerythritol triallyl ether) were below the LOD therefore the data was not suitable to measure the BCFkinetics for these two constituents. 

The study result shows that this substance is not Bioaccumulative (B) neither very Bioaccumulative (vB) and do not pass the criteria of B and vB according to ANNEX XIII of the REACH guidance document.

Key value for chemical safety assessment

BCF (aquatic species):

120 L/kg ww